CN112058245B - Organic polymer adsorbent for sewage treatment and preparation method thereof - Google Patents
Organic polymer adsorbent for sewage treatment and preparation method thereof Download PDFInfo
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- CN112058245B CN112058245B CN202011014293.0A CN202011014293A CN112058245B CN 112058245 B CN112058245 B CN 112058245B CN 202011014293 A CN202011014293 A CN 202011014293A CN 112058245 B CN112058245 B CN 112058245B
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- 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
- B01J20/265—Synthetic macromolecular compounds modified or post-treated polymers
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- 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
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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
- C02F1/28—Treatment of water, waste water, or sewage by sorption
- C02F1/285—Treatment of water, waste water, or sewage by sorption using synthetic organic sorbents
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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
- C02F2101/00—Nature of the contaminant
- C02F2101/10—Inorganic compounds
- C02F2101/103—Arsenic compounds
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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
- C02F2101/00—Nature of the contaminant
- C02F2101/10—Inorganic compounds
- C02F2101/20—Heavy metals or heavy metal compounds
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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
- C02F2101/00—Nature of the contaminant
- C02F2101/10—Inorganic compounds
- C02F2101/20—Heavy metals or heavy metal compounds
- C02F2101/22—Chromium or chromium compounds, e.g. chromates
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Abstract
The invention discloses an organic polymer adsorbent for sewage treatment, which contains praseodymium-based adsorbent, modified hyperbranched polyethyleneimine and acrylic fiber; wherein the modified hyperbranched polyethyleneimine is prepared by the following steps: dissolving polyethylenimine in deionized water, regulating pH value to 8-9, adding polyaluminum chloride, microwave reaction, filtering with 0.22 μm filter membrane, and removing filtrate to obtain the final product. The organic polymer adsorbent for sewage treatment provided by the invention is prepared by mixing praseodymium-based adsorbent, modified hyperbranched polyethyleneimine and acrylic fibers, has stable chemical properties, is environment-friendly and is suitable for As 5+ 、Cr 6+ 、Pb 2+ Has selective adsorption effect, and has special geometry and topological structure, and excellent adsorption capacity to organic pollutants such as dye and the like in sewage.
Description
Technical Field
The invention belongs to the technical field of sewage treatment, and particularly relates to an organic polymer adsorbent for sewage treatment and a preparation method thereof.
Background
Along with the continuous development of economic and social life, the human substances and living standards are continuously improved, but pollution problems are caused, and in various pollution conditions, the water pollution condition is most prominent, so that the problem of water pollution is solved. Elemental heavy metals such as lead, copper, chromium, and the like, as well as compounds and organic pollutants thereof, are widely present in domestic sewage, and these heavy metals and organic pollutants are chemically stable and cannot be biodegraded, accumulate through the food chain, and cause harm to nature and human beings.
This problem is increasingly perceived by humans and many techniques are used to remove these contaminants. The methods of coagulation and flocculation, chemical precipitation, floatation extraction, adsorption and the like of the electrochemical treatment technology are main methods for removing pollutants in water, especially dye and heavy metal pollutants, and the adsorption method has the best comprehensive performance among the methods. The choice of the type of adsorbent is critical to the efficient, rapid and stable performance of the adsorption process. Most of the organic polymer adsorbents in the prior art have the defects of short service life and poor thermal stability, and the adsorption efficiency is required to be further improved, so that an organic polymer adsorbent with more excellent performance is urgently needed.
Disclosure of Invention
In order to solve the problems, the invention provides an organic polymer adsorbent for sewage treatment and a preparation method thereof.
The technical scheme adopted for realizing the purpose of the invention is as follows:
an organic polymer adsorbent for sewage treatment comprises 25-35 parts by weight of praseodymium-based adsorbent, 88-98 parts by weight of modified hyperbranched polyethyleneimine and 140-150 parts by weight of acrylic fiber; wherein the modified hyperbranched polyethyleneimine is prepared by the following steps: dissolving polyethylenimine in deionized water, regulating pH value to 8-9, adding polyaluminum chloride, microwave reaction, filtering with 0.22 μm filter membrane, and removing filtrate to obtain the final product.
Preferably, the organic polymer adsorbent for sewage treatment comprises 28-32 parts by weight of praseodymium-based adsorbent, 90-95 parts by weight of modified hyperbranched polyethyleneimine and 144-148 parts by weight of acrylic fiber; wherein the modified hyperbranched polyethyleneimine is prepared by the following steps: dissolving polyethylenimine in deionized water, regulating pH value to 8-9, adding polyaluminum chloride, microwave reaction, filtering with 0.22 μm filter membrane, and removing filtrate to obtain the final product.
Preferably, the organic polymer adsorbent for sewage treatment comprises 30 parts by weight of praseodymium-based adsorbent, 93 parts by weight of modified hyperbranched polyethyleneimine and 146 parts by weight of acrylic fiber; wherein the modified hyperbranched polyethyleneimine is prepared by the following steps: dissolving polyethylenimine in deionized water, regulating pH value to 8-9, adding polyaluminum chloride, microwave reaction, filtering with 0.22 μm filter membrane, and removing filtrate to obtain the final product.
Specifically, in the step of preparing the modified hyperbranched polyethyleneimine, the mass ratio of the polyethyleneimine to the deionized water to the polyaluminum chloride is 5-10:30:3-5.
Specifically, in the step of preparing the modified hyperbranched polyethyleneimine, the temperature of the microwave reaction is 55-65 ℃, the power is 80-120W, and the time of the microwave reaction is 25-35min.
Specifically, the length of the acrylic fiber is 1-3cm, and the fineness is 1-5dtex.
The invention also provides a preparation method of the organic polymer adsorbent for sewage treatment, which comprises the following operation steps:
(1) According to the weight portions, mixing 30-40 portions of calcium nitrate, 20-28 portions of aluminum nitrate, 12-16 portions of praseodymium nitrate, 80-100 portions of deionized water and 10-15 portions of citric acid uniformly, heating to 75-85 ℃ and then continuously stirring until colloid is formed, naturally standing the colloid for 24 hours, drying, and finally grinding to praseodymium-based adsorbent with the average particle diameter of 0.1-0.2mm after calcination treatment;
(2) And mixing the praseodymium-based adsorbent, the modified hyperbranched polyethyleneimine, the acrylic fiber and deionized water, heating and refluxing for 5-7 hours, stopping the reaction, cooling, taking out the acrylic fiber, washing with water, and drying to obtain the organic polymer adsorbent for sewage treatment.
Specifically, in the step (1), the temperature of the drying treatment is 100 ℃, and the time of the drying treatment is 10-12 hours.
Specifically, the specific process of the calcination treatment is as follows: calcining at 350-400deg.C for 60-80min, and calcining at 750-800deg.C for 3-4 hr.
According to the technical scheme, the beneficial effects of the invention are as follows:
1) The organic polymer adsorbent for sewage treatment provided by the invention is prepared by mixing praseodymium-based adsorbent, modified hyperbranched polyethyleneimine and acrylic fibers, has stable chemical properties, is environment-friendly and is suitable for As 5+ 、Cr 6+ 、Pb 2+ Has selective adsorption effect and can be used for treating the wastewater containing As 5+ 、Cr 6+ 、Pb 2+ And also to Cu 2+ ,Cd 2+ ,Cr 3+ The method has a strong adsorption effect, and has a special geometry and a topological structure, and has excellent adsorption capacity to organic pollutants in sewage, such as dye, wherein the maximum adsorption capacity to thiophene sulfides can reach 544.37mg/g;
2) The organic polymer adsorbent prepared by the invention can be continuously used for multiple times after being recovered by simple physical (such as hydrothermal treatment) and chemical (such as ethanol, acid washing and water washing) methods after adsorbing pollutants, and can still maintain the adsorption efficiency of about 93% after being used for 10 times circularly through tests;
3) After the modified polyethylene imine is treated by the polyaluminium chloride, the thermal stability of the modified hyperbranched polyethylene imine is greatly enhanced, and the number of holes in the modified hyperbranched polyethylene imine is increased, so that the encapsulation effect on different organic pollutants and metal ions is greatly enhanced;
4) The praseodymium-based adsorbent prepared by the invention has excellent pore structure, excellent regeneration performance and As resistance 5+ 、Cr 6+ 、Pb 2+ Has excellent propertiesThe selective adsorption effect can effectively remove heavy metal ions in the sewage;
5) According to the invention, a reaction of heating reflux is adopted, so that praseodymium-based adsorbent and modified hyperbranched polyethyleneimine are filled in acrylic fibers, wherein the adhesion between the modified hyperbranched polyethyleneimine and the acrylic fibers is strong, and the modified hyperbranched polyethyleneimine and the praseodymium-based adsorbent can be coprecipitated to form a polymer in the heating reflux process, so that the modified hyperbranched polyethyleneimine is effectively filled in the acrylic fibers.
Detailed Description
Embodiments of the present invention will be described in detail below with reference to examples, but it will be understood by those skilled in the art that the following examples are only for illustrating the present invention and should not be construed as limiting the scope of the present invention. The specific conditions are not noted in the examples and are carried out according to conventional conditions or conditions recommended by the manufacturer.
Example 1
An organic polymer adsorbent for sewage treatment comprises 25 parts by weight of praseodymium-based adsorbent, 88 parts by weight of modified hyperbranched polyethyleneimine and 140 parts by weight of acrylic fiber, wherein the length of the acrylic fiber is 1cm, and the fineness is 1dtex; wherein the modified hyperbranched polyethyleneimine is prepared by the following steps: dissolving polyethylenimine in deionized water, regulating the pH value to 8, continuously adding polyaluminium chloride into the solution, placing the mixed solution into a microwave synthesizer, setting the temperature of microwave reaction to 55 ℃, carrying out microwave reaction at the power of 80W for 25min, filtering the solution by adopting a filter membrane with the thickness of 0.22 mu m, and removing the filtrate to obtain the modified hyperbranched polyethylenimine, wherein the mass ratio of polyethylenimine to deionized water to polyaluminium chloride is 5:30:3.
The preparation method of the organic polymer adsorbent for sewage treatment comprises the following operation steps:
(1) According to parts by weight, uniformly mixing 30 parts of calcium nitrate, 20 parts of aluminum nitrate, 12 parts of praseodymium nitrate, 80 parts of deionized water and 10 parts of citric acid, heating to 75 ℃, continuously stirring until colloid is formed, naturally standing the colloid for 24 hours, drying at 100 ℃ for 10 hours, and finally grinding to obtain praseodymium-based adsorbent with the average particle size of 0.1mm after calcination, wherein the specific process of the calcination is as follows: calcining at 350deg.C for 60min, and calcining at 750deg.C for 3 hr;
(2) And mixing the praseodymium-based adsorbent, the modified hyperbranched polyethyleneimine, the acrylic fiber and deionized water, heating and refluxing for 5 hours, stopping the reaction, cooling, taking out the acrylic fiber, washing with water, and drying to obtain the organic polymer adsorbent for sewage treatment.
Example 2
An organic polymer adsorbent for sewage treatment comprises 35 parts by weight of praseodymium-based adsorbent, 98 parts by weight of modified hyperbranched polyethyleneimine and 150 parts by weight of acrylic fiber, wherein the length of the acrylic fiber is 3cm, and the fineness is 5dtex; wherein the modified hyperbranched polyethyleneimine is prepared by the following steps: dissolving polyethylenimine in deionized water, regulating the pH value to 9, continuously adding polyaluminum chloride into the solution, placing the mixed solution into a microwave synthesizer, setting the microwave reaction temperature to 65 ℃ and the power to 120W for 35min, filtering the solution by adopting a filter membrane with the thickness of 0.22 mu m, and removing the filtrate to obtain the modified hyperbranched polyethylenimine, wherein the mass ratio of polyethylenimine to deionized water to polyaluminum chloride is 10:30:5.
The preparation method of the organic polymer adsorbent for sewage treatment comprises the following operation steps:
(1) According to parts by weight, 40 parts of calcium nitrate, 28 parts of aluminum nitrate, 16 parts of praseodymium nitrate, 100 parts of deionized water and 15 parts of citric acid are uniformly mixed, heated to 85 ℃, continuously stirred until colloid is formed, the colloid is naturally kept stand for 24 hours, dried at 100 ℃ for 12 hours, and finally calcined and ground to obtain the praseodymium-based adsorbent with the average particle size of 0.2mm, wherein the specific process of the calcination is as follows: calcining at 400 ℃ for 80min, and then calcining at 800 ℃ for 4 hours;
(2) And mixing the praseodymium-based adsorbent, the modified hyperbranched polyethyleneimine, the acrylic fiber and deionized water, heating and refluxing for 7 hours, stopping the reaction, cooling, taking out the acrylic fiber, washing with water, and drying to obtain the organic polymer adsorbent for sewage treatment.
Example 3
An organic polymer adsorbent for sewage treatment comprises 30 parts by weight of praseodymium-based adsorbent, 93 parts by weight of modified hyperbranched polyethyleneimine and 146 parts by weight of acrylic fiber; wherein the modified hyperbranched polyethyleneimine is prepared by the following steps: dissolving polyethylenimine in deionized water, regulating the pH value to 8-9, continuously adding polyaluminium chloride into the solution, placing the mixed solution into a microwave synthesizer, carrying out microwave reaction, filtering the solution by adopting a filter membrane with the thickness of 0.22 mu m, and removing the filtrate to obtain the modified hyperbranched polyethylenimine, wherein the mass ratio of the polyethylenimine to the deionized water to the polyaluminium chloride is 8:30:4.
The preparation method of the organic polymer adsorbent for sewage treatment comprises the following operation steps:
(1) According to parts by weight, uniformly mixing 35 parts of calcium nitrate, 24 parts of aluminum nitrate, 14 parts of praseodymium nitrate, 90 parts of deionized water and 13 parts of citric acid, heating to 80 ℃, continuously stirring until colloid is formed, naturally standing the colloid for 24 hours, drying at 100 ℃ for 11 hours, and finally grinding to obtain praseodymium-based adsorbent with the average particle size of 0.1mm after calcination, wherein the specific process of the calcination is as follows: calcining at 380 ℃ for 70min, and then calcining at 780 ℃ for 3.5 hours;
(2) And mixing the praseodymium-based adsorbent, the modified hyperbranched polyethyleneimine, the acrylic fiber and deionized water, heating and refluxing for 6 hours, stopping the reaction, cooling, taking out the acrylic fiber, washing with water, and drying to obtain the organic polymer adsorbent for sewage treatment.
Comparative example 1
In the preparation of the organic polymeric adsorbent, the modified hyperbranched polyethyleneimine was replaced with an equivalent amount of polyethyleneimine, and the rest of the operation steps were exactly the same as in example 1.
Comparative example 2
In the process of preparing the organic polymeric adsorbent, praseodymium nitrate was replaced with an equimolar amount of calcium nitrate, and the other operation steps were exactly the same as in example 2.
Organic polymeric adsorbents for wastewater treatment were prepared by the methods of examples and comparative examples, respectively, and then used for the treatment of wastewater, respectivelyAdsorption of aqueous blue X-GRRL dye solution having an initial concentration of 250mg/L and Cr 6+ The organic polymer adsorbent is circularly adsorbed for 10 times by using an aqueous solution with the ion concentration of 100mg/L, the time of each adsorption treatment is 4 hours, the mass ratio of the organic polymer adsorbent to the test solution is 1:100, the organic polymer adsorbent is cleaned by adopting ethanol and water after each adsorption, and the test results are shown in the table 1:
as can be seen from the data of example 1 and comparative example 1 in table 1, after modification treatment of polyethyleneimine with polyaluminum chloride, the thermal stability of the obtained modified hyperbranched polyethyleneimine is greatly enhanced, and the number of holes in the modified hyperbranched polyethyleneimine is increased, so that the encapsulation effect of different organic pollutants and metal ions is greatly enhanced; as can be seen from the data of example 2 and comparative example 2 in Table 1, the praseodymium-based adsorbent prepared by the present invention, the addition of praseodymium element, gives the adsorbent excellent pore structure, and is excellent in regenerability to As 5+ 、Cr 6+ 、Pb 2+ Has excellent selective adsorption effect and can effectively remove heavy metal ions in sewage.
The embodiments described above are some, but not all embodiments of the invention. The detailed description of the embodiments of the invention is not intended to limit the scope of the invention, as claimed, but is merely representative of selected embodiments of the invention. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
Claims (9)
1. An organic polymer adsorbent for sewage treatment is characterized by comprising 25-35 parts by weight of praseodymium-based adsorbent, 88-98 parts by weight of modified hyperbranched polyethyleneimine and 140-150 parts by weight of acrylic fiber;
wherein the modified hyperbranched polyethyleneimine is prepared by the following steps: dissolving polyethylenimine in deionized water, regulating the pH value to 8-9, continuously adding polyaluminium chloride into the solution, placing the mixed solution into a microwave synthesizer, carrying out microwave reaction, filtering the solution by adopting a filter membrane with the thickness of 0.22 mu m, and removing filtrate to obtain modified hyperbranched polyethylenimine;
the organic polymer adsorbent for sewage treatment is prepared by the following steps:
(1) According to the weight portions, mixing 30-40 portions of calcium nitrate, 20-28 portions of aluminum nitrate, 12-16 portions of praseodymium nitrate, 80-100 portions of deionized water and 10-15 portions of citric acid uniformly, heating to 75-85 ℃ and then continuously stirring until colloid is formed, naturally standing the colloid for 24 hours, drying, and finally grinding to praseodymium-based adsorbent with the average particle diameter of 0.1-0.2mm after calcination treatment;
(2) And mixing the praseodymium-based adsorbent, the modified hyperbranched polyethyleneimine, the acrylic fiber and deionized water, heating and refluxing for 5-7 hours, stopping the reaction, cooling, taking out the acrylic fiber, washing with water, and drying to obtain the organic polymer adsorbent for sewage treatment.
2. The organic polymer adsorbent for sewage treatment according to claim 1, which comprises 28-32 parts by weight of praseodymium-based adsorbent, 90-95 parts by weight of modified hyperbranched polyethyleneimine and 144-148 parts by weight of acrylic fiber.
3. An organic polymer adsorbent for sewage treatment according to claim 2, comprising 30 parts by weight of praseodymium-based adsorbent, 93 parts by weight of modified hyperbranched polyethyleneimine and 146 parts by weight of acrylic fiber.
4. The organic polymer adsorbent for sewage treatment according to any one of claims 1 to 3, wherein in the step of preparing the modified hyperbranched polyethyleneimine, the mass ratio of polyethyleneimine, deionized water and polyaluminum chloride is 5-10:30:3-5.
5. The organic polymer adsorbent for sewage treatment according to any one of claims 1 to 3, wherein in the step of preparing the modified hyperbranched polyethyleneimine, the temperature of the microwave reaction is 55 to 65 ℃, the power is 80 to 120W, and the time of the microwave reaction is 25 to 35min.
6. An organic polymeric adsorbent for sewage treatment according to any one of claims 1 to 3, wherein the acrylic fiber has a length of 1 to 3cm and a fineness of 1 to 5dtex.
7. A method for preparing the organic polymeric adsorbent for sewage treatment according to claim 1, comprising the following steps of:
(1) According to the weight portions, mixing 30-40 portions of calcium nitrate, 20-28 portions of aluminum nitrate, 12-16 portions of praseodymium nitrate, 80-100 portions of deionized water and 10-15 portions of citric acid uniformly, heating to 75-85 ℃ and then continuously stirring until colloid is formed, naturally standing the colloid for 24 hours, drying, and finally grinding to praseodymium-based adsorbent with the average particle diameter of 0.1-0.2mm after calcination treatment;
(2) And mixing the praseodymium-based adsorbent, the modified hyperbranched polyethyleneimine, the acrylic fiber and deionized water, heating and refluxing for 5-7 hours, stopping the reaction, cooling, taking out the acrylic fiber, washing with water, and drying to obtain the organic polymer adsorbent for sewage treatment.
8. The method for preparing an organic polymer adsorbent for sewage treatment according to claim 7, wherein in said step (1), the temperature of the drying treatment is 100 ℃, and the drying treatment time is 10 to 12 hours.
9. The method for preparing the organic polymer adsorbent for sewage treatment according to claim 7, wherein the specific process of calcination treatment is as follows: calcining at 350-400deg.C for 60-80min, and calcining at 750-800deg.C for 3-4 hr.
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