CN110721665A - Method for preparing magnetic adsorption material by using mussel shells - Google Patents
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Abstract
The invention relates to the technical field of magnetic materials, in particular to a method for preparing a magnetic adsorption material by using mussel shells. The method comprises the following steps: the method comprises the steps of grinding mussel shells serving as raw materials, adding the mussel shell powder obtained by grinding into a salt solution containing manganese ions, iron ions and zinc ions for adsorption and impregnation, filtering out mussel shell powder, adding the mussel shell powder into a deposition solution containing carbonate or bicarbonate for codeposition, filtering out solid powder, and calcining to obtain the magnetic adsorption material. The preparation method is simple and efficient; the mussel shells can be effectively and reasonably recycled; the formed magnetic adsorption material can realize good oil stain adsorption effect and is convenient to recycle.
Description
Technical Field
The invention relates to the technical field of magnetic materials, in particular to a method for preparing a magnetic adsorption material by using mussel shells.
Background
Mussel (Mytilus edulis), also known as rainbow, also called Qingkou, is a bivalve mollusk with a dark brown shell that lives on the seashore rocks. Is distributed along the coast of the yellow sea, the Bohai sea and the east sea in China. The mussel shell is wedge-shaped, the front end is sharp and thin, and the rear end is wide and round. The shell is generally 6-8 cm long, and the shell length is less than 2 times of the shell height. The shell is thin. The shell top is near the forwardmost end of the shell. The two shells are equal and symmetrical left and right, the shell surface is purple black, has luster, and has fine and obvious growth lines which grow annularly from the top.
It is a common edible shellfish and it is also processed in large quantities as "mussel", but because of its hard, inedible chitin, it produces a large amount of mussel shell waste during its consumption and processing. Generally, mussel shells are treated by simple calcination or burying, but the treatment methods cause environmental pollution and waste of resources.
Therefore, how to reasonably utilize the mussel shells is a great research hotspot for researchers in the field of marine technology. Researches show that the mussel shell has abundant fine pores, and in the calcining process, due to the decomposition of protein and calcium carbonate in the mussel shell, a large amount of gases such as carbon dioxide are formed to escape and leave pores, a more abundant hierarchical porous structure is formed, so that the specific surface area and the porosity of the mussel shell are greatly improved, and the mussel shell has a prospect of being used as an adsorbing material after being treated.
At present, the magnetic material is widely applied in the field of marine oil pollution treatment. The invention patent application of the method of immobilizing lipase Bohai Sea-9145 by magnetic Fe3O4@ SiO2-NH2 nano microspheres, which is disclosed by the Chinese patent office on 2.10.2013, is published as CN103333879A, and the method is characterized in that decomposition treatment is carried out on oil pollution in marine oil by matching a magnetic material with lipase, and then the oil removing material is recovered by a magnetic adsorption mode. However, the method of combining the magnetic material and the enzyme has great limitations, and if different oil removing materials are required to be selected or even prepared according to different oil stains, the oil stains decomposed by the enzyme still exist in the ocean, and the ocean environment is still polluted. And the adsorption mode is adopted to replace the decomposition mode, the aim of removing the marine oil stain can be achieved, the secondary pollution can be further avoided, and the oil stain can be recovered.
Disclosure of Invention
The invention provides a method for preparing a magnetic adsorption material by using mussel shells, which aims to solve a series of problems that the existing mussel shells are discarded in a large quantity and are not utilized effectively and reasonably, and the existing oil removal material for treating marine pollution is easy to generate secondary pollution and has great limitation in use. The invention aims to: firstly, simply and quickly preparing a magnetic adsorption material which can be used for marine oil removal by taking mussel shells as a raw material; secondly, the prepared magnetic adsorption material can treat oil stains in an adsorption mode, and can effectively avoid secondary pollution; and thirdly, the magnetic adsorption material is convenient to recycle after adsorbing the grease, and the magnetic material and the grease are easy to separate after recycling.
In order to achieve the purpose, the invention adopts the following technical scheme.
A method for preparing a magnetic adsorption material by using mussel shells,
the method comprises the following steps:
the method comprises the steps of grinding mussel shells serving as raw materials, adding the mussel shell powder obtained by grinding into a salt solution containing manganese ions, iron ions and zinc ions for adsorption and impregnation, filtering out mussel shell powder, adding the mussel shell powder into a deposition solution containing carbonate or bicarbonate for codeposition, filtering out solid powder, and calcining to obtain the magnetic adsorption material.
The secretion of shell protein is required for the growth of shellfish shells, so that about 5-10 wt% of protein components exist on the mussel shells actually, the protein components can collect and adsorb manganese ions, iron ions and zinc ions in a salt solution, the pores of the mussel shells after being ground can also effectively adsorb the salt solution, the manganese ions, the iron ions and the zinc ions can be adsorbed onto the mussel shell powder in the impregnation process, then the mussel shell powder is added into a deposition solution for codeposition of the metal ions, so that the metal ions form carbonate deposition and grow on the surfaces of the mussel shell powder, finally, a metal compound material layer can grow on the surfaces of the mussel shell powder by calcination treatment, the protein, calcium carbonate and the metal compounds formed by deposition can be decomposed in the calcination process to form a calcium oxide framework with rich pores, and a manganese-zinc ferrite magnetic material layer is formed on the surfaces of the calcium oxide framework, forming the magnetic adsorbent material.
As a preference, the first and second liquid crystal compositions are,
the molar ratio of manganese ions to iron ions to zinc ions in the salt solution is (45-55): (40-60): 20.
the use of manganese ions, iron ions and zinc ions in the above molar ratios facilitates the formation of the magnetic material.
As a preference, the first and second liquid crystal compositions are,
the total molar concentration of manganese ions, iron ions and zinc ions in the salt solution is 0.5-1.5 mol/L.
Too high total concentration of metal ions easily leads to the calcination in-process to form thicker and compact magnetic metal material layer on the mussel shell powder surface for the calcination decomposition of mussel shell powder itself is limited, makes its porosity still lower after calcining, and metal ion concentration is low then causes easily to be difficult to form the magnetic material layer.
As a preference, the first and second liquid crystal compositions are,
the deposition solution is saturated solution of ammonium carbonate or ammonium bicarbonate.
The saturated ammonium carbonate or saturated ammonium bicarbonate solution can achieve good deposition effect, is easy to prepare and has low cost.
As a preference, the first and second liquid crystal compositions are,
in the preparation process, one adsorption impregnation and one codeposition are taken as a cycle, and 3-5 cycles are performed in total.
Carry out a plurality of circulations and can form thicker magnetic material layer, increase final product magnetic adsorption material's particle size, make things convenient for magnetic adsorption material's recovery to the multilayer magnetic material layer also can form the gas pocket in calcining process for adsorb grease, improve grease adsorption efficiency.
As a preference, the first and second liquid crystal compositions are,
the adsorption dipping is carried out at the temperature of 40-60 ℃ for 5-10 min;
and carrying out codeposition at 5-10 ℃ for 5-10 min.
The adsorption impregnation is carried out low-temperature heating, the efficiency of the adsorption impregnation can be improved, the codeposition is carried out in a low-temperature environment, and the deposition efficiency and the deposition effect can be improved.
As a preference, the first and second liquid crystal compositions are,
the calcination treatment sequentially comprises pre-calcination treatment and high-temperature calcination treatment;
the pre-calcination treatment temperature is 600-900 ℃, and the calcination time is 2-4 h;
the high-temperature calcination treatment temperature is 1100-1200 ℃, and the calcination time is 5-8 h.
During the pre-calcination treatment, the manganese-zinc ferrite magnetic material layer can be formed firstly, calcium carbonate can be decomposed into calcium oxide, and protein can be completely decomposed. The subsequent high-temperature calcination treatment is mainly used for treating the magnetic material layer, and the magnetic conductivity, namely the magnetic property, of the magnetic material layer is improved after the high-temperature calcination treatment is carried out, so that the magnetic material layer is more convenient to recycle.
The invention has the beneficial effects that:
1) the preparation method is simple and efficient;
2) the mussel shells can be effectively and reasonably recycled;
3) the formed magnetic adsorption material can realize good oil stain adsorption effect and is convenient to recycle.
Detailed Description
The present invention will be described in further detail with reference to specific examples. Those skilled in the art will be able to implement the invention based on these teachings. Moreover, the embodiments of the present invention described in the following description are generally only some embodiments of the present invention, and not all embodiments. Therefore, all other embodiments obtained by a person of ordinary skill in the art based on the embodiments of the present invention without any creative effort shall fall within the protection scope of the present invention.
Unless otherwise specified, the raw materials used in the examples of the present invention are all commercially available or available to those skilled in the art; unless otherwise specified, the methods used in the examples of the present invention are all those known to those skilled in the art.
Example 1
A method for preparing a magnetic adsorption material by using mussel shells, which comprises the following steps:
the method comprises the following steps of grinding waste mussel shells which are separated from meat shells and are used as raw materials in a certain marine product processing plant into powder, grinding the powder until the mussel shell powder with the particle size being less than or equal to 1mm is formed, adding the obtained mussel shell powder into a salt solution prepared from manganese sulfate, ferric sulfate and zinc sulfate, and carrying out adsorption and impregnation at the temperature of 60 ℃ for 5min, wherein the molar ratio of manganese ions, iron ions and zinc ions in the salt solution is 50: 50: 20. the total molar concentration of manganese ions, iron ions and zinc ions is 0.5mol/L, then mussel shell powder is filtered and added into a saturated ammonium bicarbonate solution for codeposition for 5min at the temperature of 5 ℃, and finally solid powder is filtered and then sequentially calcined at the temperature of 600 ℃ for 4h and at the temperature of 1100 ℃ for 8h to obtain the magnetic adsorption material.
Example 2
A method for preparing a magnetic adsorption material by using mussel shells, which comprises the following steps:
the abandoned mussel shell after meat and shell separation in a certain marine product processing plant is used as a raw material for grinding, the grinding is carried out until the mussel shell powder with the particle size less than or equal to 1mm is formed, the obtained mussel shell powder is added into a salt solution prepared from manganese sulfate, ferric sulfate and zinc sulfate for adsorption and impregnation for 10min at the temperature of 40 ℃, and the molar ratio of manganese ions, iron ions and zinc ions in the salt solution is 45: 40: 20. the total molar concentration of manganese ions, iron ions and zinc ions is 1.5mol/L, then mussel shell powder is filtered and added into a saturated ammonium bicarbonate solution to carry out codeposition for 10min at the temperature of 10 ℃, one cycle of primary adsorption impregnation and primary codeposition is adopted, 3 cycles are carried out totally, and finally, after solid powder is filtered out, calcination treatment of calcining for 2 hours at the temperature of 900 ℃ and calcination treatment of calcining for 5 hours at the temperature of 1200 ℃ are carried out in sequence to obtain the magnetic adsorption material.
Example 3
A method for preparing a magnetic adsorption material by using mussel shells, which comprises the following steps:
the abandoned mussel shell after meat and shell separation in a certain marine product processing plant is used as a raw material for grinding, the grinding is carried out until the mussel shell powder with the particle size less than or equal to 1mm is formed, the obtained mussel shell powder is added into a salt solution prepared from manganese sulfate, ferric sulfate and zinc sulfate for adsorption and impregnation for 10min at the temperature of 50 ℃, and the molar ratio of manganese ions, iron ions and zinc ions in the salt solution is 55: 60: 20. the total molar concentration of manganese ions, iron ions and zinc ions is 1.0mol/L, then mussel shell powder is filtered and added into a saturated ammonium bicarbonate solution to carry out codeposition for 10min at the temperature of 5 ℃, one cycle of primary adsorption impregnation and primary codeposition is adopted, 5 cycles are carried out totally, and finally solid powder is filtered out and then sequentially calcined at the temperature of 800 ℃ for 4 hours and calcined at the temperature of 1200 ℃ for 6 hours, so that the magnetic adsorption material is obtained.
Example 4
A method for preparing a magnetic adsorption material by using mussel shells, which comprises the following steps:
the abandoned mussel shell after meat and shell separation in a certain marine product processing plant is used as a raw material for grinding, the grinding is carried out until the mussel shell powder with the particle size less than or equal to 1mm is formed, the obtained mussel shell powder is added into a salt solution prepared from manganese sulfate, ferric sulfate and zinc sulfate for adsorption and impregnation for 10min at the temperature of 50 ℃, and the molar ratio of manganese ions, iron ions and zinc ions in the salt solution is 55: 52: 20. the total molar concentration of manganese ions, iron ions and zinc ions is 1.5mol/L, then mussel shell powder is filtered out and added into a saturated ammonium bicarbonate solution to carry out codeposition for 10min at the temperature of 10 ℃, one cycle of primary adsorption impregnation and primary codeposition is adopted, 3 cycles are carried out totally, and finally, after solid powder is filtered out, calcination treatment of calcination at the temperature of 800 ℃ for 3 hours and calcination at the temperature of 1200 ℃ for 8 hours is carried out in sequence, so that the magnetic adsorption material can be obtained.
Example 5
A method for preparing a magnetic adsorption material by using mussel shells, which comprises the following steps:
the abandoned mussel shell after meat and shell separation in a certain marine product processing plant is used as a raw material for grinding, the grinding is carried out until the mussel shell powder with the particle size less than or equal to 1mm is formed, the obtained mussel shell powder is added into a salt solution prepared from manganese sulfate, ferric sulfate and zinc sulfate for adsorption and impregnation for 10min at the temperature of 55 ℃, and the molar ratio of manganese ions, iron ions and zinc ions in the salt solution is 55: 50: 20. the total molar concentration of manganese ions, iron ions and zinc ions is 1.0mol/L, then mussel shell powder is filtered and added into a saturated ammonium bicarbonate solution to carry out codeposition for 10min at the temperature of 5 ℃, one cycle of primary adsorption impregnation and primary codeposition is adopted, 4 cycles are carried out totally, and finally solid powder is filtered out and then sequentially calcined at the temperature of 800 ℃ for 3 hours and calcined at the temperature of 1200 ℃ for 6 hours, so that the magnetic adsorption material is obtained.
Detection 1:
the magnetic recovery test was performed on the magnetic adsorbent obtained in examples 1 to 5;
50g of each of the magnetic adsorbents obtained in examples 1 to 5 was dispersed in 300mL of ethyl acetate, and after standing for 10min, the magnetic adsorbent was recovered by a flat electromagnet, and after recovery, the magnetic adsorbent was calcined at 600 ℃ for 2 hours and weighed, and the recovery rate of the magnetic adsorbent was calculated from the remaining weight. The recovery rate of the magnetic adsorption material prepared in example 1 was calculated to be 82.61%, and the recovery rate of the magnetic adsorption material prepared in examples 2 to 5 was calculated to be 92.62-94.11%.
And (3) detection 2:
the magnetic adsorbent obtained in examples 2 to 5 was subjected to an oil absorption test;
respectively dispersing 5g of the magnetic adsorption material prepared in the embodiments 2 to 5 in 100mL of ethyl acetate, standing and adsorbing for 30min, controlling a flat electromagnet in the standing and adsorbing process to enable the magnetic adsorption material to be suspended in the ethyl acetate and not to be deposited to the bottom, increasing the magnetic field of the flat electromagnet after the standing and adsorbing process is finished, magnetically adsorbing and recovering the magnetic adsorption material, respectively measuring the volume of the residual ethyl acetate, and calculating the oil and fat amount which can be adsorbed by the magnetic adsorption material. The amount of oil and fat adsorbed by the magnetic adsorbing material prepared in each gram of the embodiment 2 to 5 is calculated to be about 1.02-1.16 mL.
And (3) detection:
5g of the magnetic adsorbents obtained in examples 2 to 5 were dispersed in a volume ratio of oil to water of 1: 1, the total volume of the layered solution is 100mL, the magnetic adsorption material firstly adsorbs the ethyl acetate through an oil layer, and gradually sinks, when the magnetic adsorption material sinks to the oil-water interface, because the magnetic adsorption material is coated by oil drops, most of the magnetic adsorption material stays at the oil-water interface and does not sink any more, and because the oil drops are not coated completely, a small amount of the magnetic adsorption material further sinks, but the calcium oxide skeleton is dissolved in the sinking process, the particles are reduced, and the insoluble magnetic material layer coated by the oil drops rises to the oil-water interface, the method can predict that the magnetic adsorption material can always exist at an oil-water interface and is not deposited to the seabed in the actual seawater oil removal application process, is very convenient to recover, and after the flat electromagnet is utilized to adsorb and recover the magnetic adsorption material, and the volume of the oil layer is reduced by about 9.6-10.2% through measurement again, and a good oil absorption effect can be realized.
Claims (7)
1. A method for preparing a magnetic adsorption material by using mussel shells is characterized in that,
the method comprises the following steps:
the method comprises the steps of grinding mussel shells serving as raw materials, adding the mussel shell powder obtained by grinding into a salt solution containing manganese ions, iron ions and zinc ions for adsorption and impregnation, filtering out mussel shell powder, adding the mussel shell powder into a deposition solution containing carbonate or bicarbonate for codeposition, filtering out solid powder, and calcining to obtain the magnetic adsorption material.
2. The method for preparing magnetic adsorption material by using mussel shell as claimed in claim 1,
the molar ratio of manganese ions to iron ions to zinc ions in the salt solution is (45-55): (40-60): 20.
3. the method for preparing magnetic adsorption material by using mussel shell as claimed in claim 1 or 2,
the total molar concentration of manganese ions, iron ions and zinc ions in the salt solution is 0.5-1.5 mol/L.
4. The method for preparing magnetic adsorption material by using mussel shell as claimed in claim 1,
the deposition solution is saturated solution of ammonium carbonate or ammonium bicarbonate.
5. The method for preparing magnetic adsorption material by using mussel shell as claimed in claim 1,
in the preparation process, one adsorption impregnation and one codeposition are taken as a cycle, and 3-5 cycles are performed in total.
6. The method for preparing magnetic adsorption material by using mussel shell as claimed in claim 1 or 5,
the adsorption dipping is carried out at the temperature of 40-60 ℃ for 5-10 min;
and carrying out codeposition at 5-10 ℃ for 5-10 min.
7. The method for preparing magnetic adsorption material by using mussel shell as claimed in claim 1,
the calcination treatment sequentially comprises pre-calcination treatment and high-temperature calcination treatment;
the pre-calcination treatment temperature is 600-900 ℃, and the calcination time is 2-4 h;
the high-temperature calcination treatment temperature is 1100-1200 ℃, and the calcination time is 5-8 h.
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| CN111821951A (en) * | 2020-07-06 | 2020-10-27 | 杭州电子科技大学 | Recyclable nitrogen and phosphorus synchronous adsorbent and preparation method and application thereof |
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