CN105771876A - Preparation method of modified eggshell magnetic adsorbent and method for removing heavy metal in water - Google Patents
Preparation method of modified eggshell magnetic adsorbent and method for removing heavy metal in water Download PDFInfo
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- CN105771876A CN105771876A CN201610333371.0A CN201610333371A CN105771876A CN 105771876 A CN105771876 A CN 105771876A CN 201610333371 A CN201610333371 A CN 201610333371A CN 105771876 A CN105771876 A CN 105771876A
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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
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/04—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising compounds of alkali metals, alkaline earth metals or magnesium
- B01J20/043—Carbonates or bicarbonates, e.g. limestone, dolomite, aragonite
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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
- B01J20/28002—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 physical properties
- B01J20/28009—Magnetic properties
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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
- C02F1/281—Treatment of water, waste water, or sewage by sorption using inorganic sorbents
Abstract
The invention provides a preparation method of a modified eggshell magnetic adsorbent and a method for removing heavy metal in water. With domestic waste, eggshell, as a raw material, the eggshell is endowed with magnetism through chemical and physical modification, and the magnetic adsorbent, which is cheap, excellent, stable, environmentally friendly and easy to recycle and is capable of adsorbing heavy metal wastewater, is obtained. According to the preparation method, the technical problems that the heavy metal wastewater is difficult to treat at present and a treatment reagent or material is high in price, poor in effect, complicated in preparation technology and difficult to recycle, and easily causes secondary pollution are solved; and the method has relatively high practical value.
Description
Technical field
The invention belongs to changing waste into resources to utilize and water-treatment technology field, be specifically related to the preparation method of a kind of modified eggshell magnetic adsorbent and remove the method for heavy metal in water.
Background technology
Along with the development of growth in the living standard and food service industry, the people need to consume substantial amounts of fowl egg in daily life, and eggshell is as a kind of garbage, it is typically with landfill disposal, easily causing serious environmental pollution, and the main component of eggshell is calcium carbonate, its Exploitative potential is very big.And utilize eggshell to do adsorbent to process heavy metal wastewater thereby, it it is the problem of a lot of people's researchs at present, name is called a kind of eggshell heavy metal ion adsorbent and preparation method thereof, the patent No. is in the patent document of 201210119055, describing the preparation method utilizing eggshell as adsorbent for heavy metal, the method removes inner membrance after being soaked in aqueous slkali by eggshell, then washes, filters, insert after drying baker is dried in heat-treatment furnace and calcine, then cool down.Adopt the adsorbent that the method is made, although having certain absorption property, but adsorption efficiency is low, adsorbent is difficult to reclaim, it is impossible to recycling, it is therefore necessary to propose to improve.
Summary of the invention
Present invention solves the technical problem that: the method for heavy metal in the preparation method of a kind of modified eggshell magnetic adsorbent and removal water, utilize domestic refuse eggshell as raw material, obtain cheap, excellent, stable, environmental protection and the heavy metal wastewater thereby absorption magnetic environment material being easily recycled by chemically and physically modified its magnetic that gives, there is higher practical value.
The technical solution used in the present invention: the preparation method of modified eggshell magnetic adsorbent, comprises following step:
1) chemical modification of eggshell: the eggshell of collection is concentrated and washes, it is then placed in drying baker and heats to 60 DEG C-80 DEG C drying, dried eggshell pulverized 80-120 mesh sieve, egg-shell meal and water soak in 1:2 ratio and add the modifying agent of egg-shell meal weight 5%, by 150-180 turn/the speed concussion 1.5-2h of min obtains modified eggshell solution；
2) preparation of product in the middle of eggshell: iron salt is added and fully dissolves to obtain iron salt solutions in deionized water, then ferrous salt is added in iron salt solutions and fully dissolve to obtain mixed solution, mixed solution heated to 50 DEG C-60 DEG C and turn/speed stirring reaction about the 30min of min by 400-800, modified eggshell solution is added in mixed solution and obtain eggshell solution, with 5% aqueous slkali, the pH value of eggshell solution is adjusted to 9-10, then heat to 70 DEG C-80 DEG C, and turn/speed stirring reaction about the 2h of min by 400-800, directly filter to obtain filter product, then alternately wash filter product to neutrality to heat to 60 DEG C-80 DEG C to dry with clear water and ethanol and to obtain product in the middle of eggshell, above-mentioned steps all carries out under inert gas shielding；
3) physical modification: put in Muffle furnace and be filled with noble gas by product in the middle of eggshell, heats and takes out after being incubated about 2h to 450 DEG C-540 DEG C, cool down the magnetic adsorbent that gets product under room temperature.
Above-mentioned steps 1) in, described modifying agent is zinc chloride, magnesium chloride or both mixture, and when for both mixture, the mixed proportion of described zinc chloride and magnesium chloride is 1:2.
Above-mentioned steps 2) in, the additional proportion of described iron salt and ferrous salt is 1:2, and both ratios with deionized water are 1:20.
Above-mentioned steps 2) in, in described eggshell solution, the ratio of modified eggshell solution and mixed solution is 2:3.
Above-mentioned steps 2) and step 3) in, described noble gas is nitrogen.
Above-mentioned steps 2) in, described aqueous slkali is sodium hydroxide or ammonia.
Also provide for a kind of modified eggshell magnetic adsorbent and remove the method for heavy metal in water, comprise following step:
1) pH value making heavy metal wastewater thereby is maintained at acid state；
2) the finished product magnetic adsorbent obtained is added in heavy metal wastewater thereby in 1～2.5:50 ratio, stirring at normal temperature adsorption reaction 1h, make the impurity absorption in heavy metal wastewater thereby on finished product magnetic adsorbent；
3) being banished by the supernatant in wastewater disposal basin to sedimentation tank, additional Magnet will be adsorbed with the finished product magnetic adsorbent sucking-off of impurity, continue to recycle after removing impurity thereon.
Present invention advantage compared with prior art:
1, for current heavy metal containing wastewater treatment difficulty, reagent treatment or material price height, weak effect, recovery difficulty, can not reuse, easily cause secondary pollution problems, utilize domestic refuse Ovum crusta Gallus domesticus as raw material, modifiied by chemically and physically method and load magnetic, obtain the magnetic environment material that heavy metal in waste water is had good adsorbent performance, reached to turn waste into wealth, the purpose of the treatment of wastes with processes of wastes against one another, reduce wastewater treatment expense；
2, the magnetic material that the present invention obtains, overcomes adsorbing material and reclaims a difficulty difficult problem and recycling capable of circulation；
3, add zinc chloride and the modified microstructure that can change material through high-temperature calcination of magnesium chloride, increase its porosity, improve its absorption property；
4, the magnetic material that the present invention obtains, non-secondary pollution risk in application process.
Detailed description of the invention
Embodiments of the invention are described below.
Embodiment one: the preparation method of modified eggshell magnetic adsorbent, comprises following step:
1) chemical modification of eggshell: the eggshell of collection is concentrated and washes, it is then placed in drying baker and heats to 60 DEG C of drying, dried eggshell pulverized 80 mesh sieves, egg-shell meal and water soak in 1:2 ratio and add the modifying agent of egg-shell meal weight 5%, shaking 1.5h by the speed of 150 turns/min and obtain modified eggshell solution, above-mentioned modifying agent is zinc chloride.
2) preparation of product in the middle of eggshell: iron salt is added and fully dissolves to obtain iron salt solutions in deionized water, then ferrous salt is added in iron salt solutions and fully dissolve to obtain mixed solution, the additional proportion of above-mentioned iron salt and ferrous salt is 1:2, and both ratios with deionized water are 1:20；Being heated by mixed solution to 50 DEG C and by speed stirring reaction about the 30min of 400 turns/min, added by modified eggshell solution in mixed solution and obtain eggshell solution, in described eggshell solution, the ratio of modified eggshell solution and mixed solution is 2:3；With 5% sodium hydroxide solution, the pH value of eggshell solution is adjusted to 9; then heat to 70 DEG C; and by speed stirring reaction about the 2h of 400 turns/min; directly filter to obtain filter product; then alternately washing filter product to neutrality to heat to 60 DEG C to dry with clear water and ethanol and to obtain product in the middle of eggshell, above-mentioned steps carries out all under nitrogen protection；
3) physical modification: put in Muffle furnace and be filled with nitrogen by product in the middle of eggshell, heats and takes out after being incubated about 2h to 450 DEG C, cool down the magnetic adsorbent that gets product under room temperature.
Embodiment two: the preparation method of modified eggshell magnetic adsorbent, comprises following step:
1) chemical modification of eggshell: the eggshell of collection is concentrated and washes, it is then placed in drying baker and heats to 80 DEG C of drying, dried eggshell pulverized 120 mesh sieves, egg-shell meal and water soak in 1:2 ratio and add the modifying agent of egg-shell meal weight 5%, described modifying agent is magnesium chloride, shakes 2h by the speed of 180 turns/min and obtains modified eggshell solution；
2) preparation of product in the middle of eggshell: iron salt is added and fully dissolves to obtain iron salt solutions in deionized water, then ferrous salt is added in iron salt solutions and fully dissolve to obtain mixed solution, the additional proportion of above-mentioned iron salt and ferrous salt is 1:2, and both ratios with deionized water are 1:20；Being heated by mixed solution to 60 DEG C and by speed stirring reaction about the 30min of 800 turns/min, added by modified eggshell solution in mixed solution and obtain eggshell solution, in described eggshell solution, the ratio of modified eggshell solution and mixed solution is 2:3；With 5% ammonia, the pH value of eggshell solution is adjusted to 10; then heat to 80 DEG C; and by speed stirring reaction about the 2h of 800 turns/min; directly filter to obtain filter product; then alternately washing filter product to neutrality to heat to 80 DEG C to dry with clear water and ethanol and to obtain product in the middle of eggshell, above-mentioned steps all carries out under argon shield；
3) physical modification: put in Muffle furnace and be filled with argon by product in the middle of eggshell, heats and takes out after being incubated about 2h to 540 DEG C, cool down the magnetic adsorbent that gets product under room temperature.
Embodiment three: the preparation method of modified eggshell magnetic adsorbent, comprises following step:
1) chemical modification of eggshell: the eggshell of collection is concentrated and washes, it is then placed in drying baker and heats to 70 DEG C of drying, dried eggshell pulverized 100 mesh sieves, egg-shell meal and water soak in 1:2 ratio and add the modifying agent of egg-shell meal weight 5%, described modifying agent is the mixture of zinc chloride and magnesium chloride, and the mixed proportion of zinc chloride and magnesium chloride is 1:2, then obtain modified eggshell solution by the speed concussion 1.8h of 160 turns/min；
2) preparation of product in the middle of eggshell: iron salt is added and fully dissolves to obtain iron salt solutions in deionized water, then ferrous salt is added in iron salt solutions and fully dissolve to obtain mixed solution, the additional proportion of described iron salt and ferrous salt is 1:2, and both ratios with deionized water are 1:20；Mixed solution is heated to 55 DEG C and by speed stirring reaction about the 30min of 600 turns/min; modified eggshell solution is added in mixed solution and obtain eggshell solution; the ratio of modified eggshell solution and mixed solution is 2:3; the pH value of eggshell solution is adjusted to 8 by the sodium hydroxide with 5%; then heat to 75 DEG C; and by speed stirring reaction about the 2h of 600 turns/min; directly filter to obtain filter product; then alternately washing filter product to neutrality to heat to 70 DEG C to dry with clear water and ethanol and to obtain product in the middle of eggshell, above-mentioned steps carries out all under nitrogen protection；
3) physical modification: put in Muffle furnace and be filled with nitrogen by product in the middle of eggshell, heats and takes out after being incubated about 2h to 500 DEG C, cool down the magnetic adsorbent that gets product under room temperature.
Utilize above-mentioned modified eggshell magnetic adsorbent to remove the method for heavy metal in water, comprise following step:
1) pH making heavy metal wastewater thereby is maintained at 3～6；
2) by the finished product magnetic adsorbent that obtains by 1～2.5:50 ratio addition heavy metal wastewater thereby, 30min～1h, what make in waste water is heavy metal ion adsorbed on finished product magnetic adsorbent；
3) reaction upon adsorption terminates, supernatant in wastewater disposal basin is banished to sedimentation tank, after the finished product magnetic adsorbent being adsorbed with heavy metal pollution ion being adsorbed in sedimentation tank pool wall by additional Magnet, discharge clear liquid, reclaim the adsorbent being adsorbed with heavy metal pollution ion, and continue to recycle with after drying at 60 DEG C-80 DEG C after the acid solution vibration desorption of 0.5%～1%.
Above-described embodiment, simply presently preferred embodiments of the present invention, not for limiting the scope of the present invention, therefore all equivalence changes done with content described in the claims in the present invention, all should include within the claims in the present invention scope.
Claims (7)
1. the preparation method of modified eggshell magnetic adsorbent, it is characterised in that comprise following step:
1) chemical modification of eggshell: the eggshell of collection is concentrated and washes, it is then placed in drying baker and heats to 60 DEG C-80 DEG C drying, dried eggshell pulverized 80-120 mesh sieve, egg-shell meal and water soak in 1:2 ratio and add the modifying agent of egg-shell meal weight 5%, by 150-180 turn/the speed concussion 1.5-2h of min obtains modified eggshell solution；
2) preparation of product in the middle of eggshell: iron salt is added and fully dissolves to obtain iron salt solutions in deionized water, then ferrous salt is added in iron salt solutions and fully dissolve to obtain mixed solution, mixed solution heated to 50 DEG C-60 DEG C and turn/speed stirring reaction about the 30min of min by 400-800, modified eggshell solution is added in mixed solution and obtain eggshell solution, with 5% aqueous slkali, the pH value of eggshell solution is adjusted to 9-10, then heat to 70 DEG C-80 DEG C, and turn/speed stirring reaction about the 2h of min by 400-800, directly filter to obtain filter product, then after alternately filter product being washed till neutrality with clear water and ethanol, the middle product of eggshell are dried to obtain at 60 DEG C-80 DEG C, above-mentioned steps all carries out under inert gas shielding；
3) physical modification: put in Muffle furnace and be filled with noble gas by product in the middle of eggshell, heats and takes out after being incubated about 2h to 450 DEG C-540 DEG C, cool down the magnetic adsorbent that gets product under room temperature.
2. the preparation method of modified eggshell magnetic adsorbent according to claim 1, it is characterized in that: above-mentioned steps 1) in, described modifying agent is zinc chloride, magnesium chloride or both mixture, and when for both mixture, the mixed proportion of described zinc chloride and magnesium chloride is 1:2.
3. the preparation method of modified eggshell magnetic adsorbent according to claim 1, it is characterised in that: above-mentioned steps 2) in, the additional proportion of described iron salt and ferrous salt is 1:2, and both ratios with deionized water are 1:20.
4. the preparation method of modified eggshell magnetic adsorbent according to claim 1, it is characterised in that: above-mentioned steps 2) in, in described eggshell solution, the ratio of modified eggshell solution and mixed solution is 2:3.
5. the preparation method of modified eggshell magnetic adsorbent according to claim 1, it is characterised in that: above-mentioned steps 2) and step 3) in, described noble gas is nitrogen or argon.
6. the preparation method of modified eggshell magnetic adsorbent according to claim 1, it is characterised in that: above-mentioned steps 2) in, described aqueous slkali is sodium hydroxide or ammonia.
7. utilize the modified eggshell magnetic adsorbent described in claim 1-6 to remove the method for heavy metal in water, it is characterised in that to comprise following step:
1) pH making heavy metal wastewater thereby is maintained at 3～6；
2) by the finished product magnetic adsorbent that obtains by 1～2.5:50 ratio addition heavy metal wastewater thereby, stirring at normal temperature adsorption reaction 30min～1h, what make in waste water is heavy metal ion adsorbed on finished product magnetic adsorbent；
3) reaction upon adsorption terminates, supernatant in wastewater disposal basin is banished to sedimentation tank, after the finished product magnetic adsorbent being adsorbed with heavy metal pollution ion being adsorbed in sedimentation tank pool wall by additional Magnet, discharge clear liquid, reclaim the adsorbent being adsorbed with heavy metal pollution ion, and continue to recycle with after drying at 60 DEG C-80 DEG C after the acid solution vibration desorption of 0.5%～1%.
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106362654A (en) * | 2016-10-08 | 2017-02-01 | 江苏大学 | Method for preparing imprinted beads from stable magnetic egg shell powder through Pickering emulsion polymerization technology |
| CN106925233A (en) * | 2017-05-16 | 2017-07-07 | 宝鸡文理学院 | The preparation of the useless modified dephosphorization magnetic adsorptive material of eggshell and the minimizing technology of phosphorus in water |
| CN107686146A (en) * | 2017-09-12 | 2018-02-13 | 南京国龙生物科技有限公司 | A kind of handling process of aquaculture heavy metal in waste water copper |
| CN109926024A (en) * | 2019-03-27 | 2019-06-25 | 湖南工学院 | A kind of preparation method and applications of magnetism organic modified nano adsorbent material |
| CN110404500A (en) * | 2019-06-18 | 2019-11-05 | 江门市泰汇环保科技有限公司 | A kind of multiple-effect compound type sewage-treating agent and preparation method thereof |
| CN110877921A (en) * | 2019-08-28 | 2020-03-13 | 齐鲁理工学院 | Method for removing total nitrogen in water by using modified eggshells |
| CN111644159A (en) * | 2020-05-25 | 2020-09-11 | 哈尔滨工业大学 | Magnetic adsorbent based on modified eggshell and preparation method and application thereof |
| CN116440866A (en) * | 2023-03-13 | 2023-07-18 | 武汉工程大学 | Preparation method and application of three-dimensional spongy porous heavy metal ion adsorbent based on activated eggshells |
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Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106362654A (en) * | 2016-10-08 | 2017-02-01 | 江苏大学 | Method for preparing imprinted beads from stable magnetic egg shell powder through Pickering emulsion polymerization technology |
| CN106362654B (en) * | 2016-10-08 | 2019-04-02 | 江苏大学 | A kind of method that the Pickering emulsion polymerization technology that magnetism egg-shell meal is stable prepares trace microballoon |
| CN106925233A (en) * | 2017-05-16 | 2017-07-07 | 宝鸡文理学院 | The preparation of the useless modified dephosphorization magnetic adsorptive material of eggshell and the minimizing technology of phosphorus in water |
| CN107686146A (en) * | 2017-09-12 | 2018-02-13 | 南京国龙生物科技有限公司 | A kind of handling process of aquaculture heavy metal in waste water copper |
| CN109926024A (en) * | 2019-03-27 | 2019-06-25 | 湖南工学院 | A kind of preparation method and applications of magnetism organic modified nano adsorbent material |
| CN109926024B (en) * | 2019-03-27 | 2022-03-01 | 湖南工学院 | Preparation method and application of magnetic organic modified nano adsorption material |
| CN110404500A (en) * | 2019-06-18 | 2019-11-05 | 江门市泰汇环保科技有限公司 | A kind of multiple-effect compound type sewage-treating agent and preparation method thereof |
| CN110877921A (en) * | 2019-08-28 | 2020-03-13 | 齐鲁理工学院 | Method for removing total nitrogen in water by using modified eggshells |
| CN111644159A (en) * | 2020-05-25 | 2020-09-11 | 哈尔滨工业大学 | Magnetic adsorbent based on modified eggshell and preparation method and application thereof |
| CN116440866A (en) * | 2023-03-13 | 2023-07-18 | 武汉工程大学 | Preparation method and application of three-dimensional spongy porous heavy metal ion adsorbent based on activated eggshells |
| CN116440866B (en) * | 2023-03-13 | 2023-09-22 | 武汉工程大学 | Preparation method and application of three-dimensional spongy porous heavy metal ion adsorbent based on activated eggshells |
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