CN109794224A - A kind of heavy metal chelant Fe3O4The preparation method of Chitosan Composites - Google Patents

A kind of heavy metal chelant Fe3O4The preparation method of Chitosan Composites Download PDF

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Publication number
CN109794224A
CN109794224A CN201910054492.5A CN201910054492A CN109794224A CN 109794224 A CN109794224 A CN 109794224A CN 201910054492 A CN201910054492 A CN 201910054492A CN 109794224 A CN109794224 A CN 109794224A
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China
Prior art keywords
solution
chitosan
heavy metal
preparation
chitosan composites
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CN201910054492.5A
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Chinese (zh)
Inventor
陈新
陈亿军
薛强
张少华
王平
奉向东
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Wuhan Institute of Rock and Soil Mechanics of CAS
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Wuhan Institute of Rock and Soil Mechanics of CAS
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Abstract

The invention belongs to environmental protection technical fields, disclose a kind of heavy metal chelant Fe3O4The preparation method of Chitosan Composites, comprising: chitosan is dissolved in aqueous acetic acid, with obtained solution A;Wherein, the concentration range of the solution A is 1g/L~30g/L, and in the aqueous acetic acid, the range of the volume ratio of acetic acid and water is 1:100~3:100;By FeCl3·6H2O and FeCl2·4H2O is dissolved in distilled water, with obtained solution B;Wherein, the concentration of ferric ion and ferrous ion ratio is 2:1, and the concentration range of the ferric ion is 0.1mol/L~1mol/L;Alkaline solution and the solution A are sequentially added in the solution B, with obtained solution C;The pH value of solution C is adjusted, and is heated, is kept the temperature, and resulting black product is washed with deionized water and dehydrated alcohol respectively, it is dry, obtain Fe3O4Chitosan Composites.Method provided by the invention is able to suppress the toxicity damage of process, and guarantees chelate stability, and simple process is efficient.

Description

A kind of heavy metal chelant Fe3O4The preparation method of Chitosan Composites
Technical field
The present invention relates to environmental protection technical field, in particular to a kind of heavy metal chelant Fe3O4Chitosan Composites Preparation method.
Background technique
Heavy metal chelant Fe3O4Chitosan Composites are widely applied in the harmless treatment of incineration of refuse flyash, energy Enough good chelating heavy metal ion.But since chitosan is poor to low-concentration heavy metal ions adsorptivity, adsorptive selectivity Difference, the disadvantages of time of equilibrium adsorption is longer;In the prior art, this problem is solved often through chemical modification.But it is chemical It includes that the crosslinking agent of the volatile reagents such as toxic glutaraldehyde, epoxychloropropane is stablized to improve chitosan that addition is needed in modification Property, to human body and environmental pollution in preparation process.
Summary of the invention
The present invention provides a kind of heavy metal chelant Fe3O4The preparation method of Chitosan Composites solves in the prior art Heavy metal chelant Fe3O4Crosslinking agent easily leads to the problem of human body and environmental nuisance in Chitosan Composites preparation process.
In order to solve the above technical problems, the present invention provides a kind of heavy metal chelant Fe3O4The system of Chitosan Composites Preparation Method, comprising:
Chitosan is dissolved in aqueous acetic acid, with obtained solution A;Wherein, the concentration range of the solution A be 1g/L~ 30g/L, in the aqueous acetic acid, the range of the volume ratio of acetic acid and water is 1:100~3:100;
By FeCl3·6H2O and FeCl2·4H2O is dissolved in distilled water, with obtained solution B;Wherein, ferric ion and two The concentration ratio of valence iron ion is 2:1, and the concentration range of the ferric ion is 0.1mol/L~1mol/L;
Alkaline solution and the solution A are sequentially added in the solution B, with obtained solution C;
The pH value of solution C is adjusted, and is heated, is kept the temperature, and resulting black product is used into deionized water and nothing respectively Water-ethanol washing, it is dry, obtain Fe3O4Chitosan Composites.
Further, the alkaline solution is industrial ammonia or sodium hydrate aqueous solution.
Further, the pH value range of the solution C is 8~10.
Further, the temperature range of heating is 60 DEG C~80 DEG C.
Further, the time range of heat preservation is 3h~10h.
Further, the Fe3O4In Chitosan Composites, Fe3O4Than range it is 1:1~1 with the quality of chitosan: 4。
One or more technical solutions provided in the embodiments of the present application have at least the following technical effects or advantages:
The heavy metal chelant Fe provided in the embodiment of the present application3O4The preparation method of Chitosan Composites, by chitosan It is dissolved in acetum, by controlling the aqueous acetic acid concentration of chitosan in 1g/L~30g/L, the volume ratio of acetic acid and water For 1:100~3:100, to increase the dissolubility of chitosan, and the viscosity and stability of chitosan is kept, chitosan is avoided to occur The phenomenon that self aggregation;It is added and keeps Fe3O4The FeCl of particle dispersing uniformity3·6H2O and FeCl2·4H2O source of iron, forming component Uniform Fe3O4/ Chitosan Composites;And pH value of solution is adjusted, heating and thermal insulation improves reaction rate, prepares high-efficiency and economic environmental protection Heavy metal chelant;Meanwhile, it is capable to which substituting crosslinking agent guarantees product Fe3O4The stability of Chitosan Composites, to control life Toxicity damage during production.And preparation process is simple, safety and environmental protection, avoids causing to damage to environment and human body, has extensive Application prospect and Practical significance.
Specific embodiment
The embodiment of the present application is by providing a kind of heavy metal chelant Fe3O4The preparation method of Chitosan Composites solves Heavy metal chelant Fe in the prior art3O4Crosslinking agent easily leads to human body and environmental nuisance in Chitosan Composites preparation process The problem of.
In order to better understand the above technical scheme, below in conjunction with specification and specific embodiment to above-mentioned skill Art scheme is described in detail, it should be understood that the specific features in the embodiment of the present invention and embodiment are to present techniques side The detailed description of case, rather than the restriction to technical scheme, in the absence of conflict, the embodiment of the present application and Technical characteristic in embodiment can be combined with each other.
A kind of heavy metal chelant Fe3O4The preparation method of Chitosan Composites, comprising:
Chitosan is dissolved in aqueous acetic acid, with obtained solution A;Wherein, the concentration range of the solution A be 1g/L~ 30g/L, in the aqueous acetic acid, the range of the volume ratio of acetic acid and water is 1:100~3:100;By controlling chitosan water The volume ratio of solution concentration and acetic acid and water to increase the dissolubility of chitosan, and keeps the viscosity and stability of chitosan, keeps away Exempt from chitosan and the phenomenon that self aggregation occurs.
By FeCl3·6H2O and FeCl2·4H2O is dissolved in distilled water, with obtained solution B;Wherein, ferric ion and two The concentration ratio of valence iron ion is 2:1, and the concentration range of the ferric ion is 0.1mol/L~1mol/L;Forming component is uniform Fe3O4/ Chitosan Composites.
Alkaline solution and the solution A are sequentially added in the solution B, with obtained solution C;
The pH value of solution C is adjusted, and is heated, is kept the temperature, and resulting black product is used into deionized water and nothing respectively Water-ethanol washing, it is dry, obtain Fe3O4Chitosan Composites.
It is worth noting that this method preparation process is simple, without adding volatile toxic substance as crosslinking agent, former material Expect that safety and environmental protection is pollution-free, lower temperature control comparatively fast generates reaction rate, good economy performance, the composite material partial size of generation is small, Large specific surface area, Fe3O4It is suitable with the mass ratio of chitosan, it ensure that extensive suction of the chitosan to heavy metal ion in flying dust It is attached, and realize Fe3O4To As3+、As5+Deng the selective absorption having compared with strong cytotoxicity, the ion of neurotoxicity, using wide It is general.
Further, the alkaline solution is industrial ammonia or sodium hydrate aqueous solution.
Further, the pH value range of the solution C is 8~10.
Further, the temperature range of heating is 60 DEG C~80 DEG C.
Further, the time range of heat preservation is 3h~10h.
Further, the Fe3O4In Chitosan Composites, Fe3O4Than range it is 1:1~1 with the quality of chitosan: 4。
One or more technical solutions provided in the embodiments of the present application have at least the following technical effects or advantages:
The heavy metal chelant Fe provided in the embodiment of the present application3O4The preparation method of Chitosan Composites, by chitosan It is dissolved in acetum, by controlling the aqueous acetic acid concentration of chitosan in 1g/L~30g/L, the volume ratio of acetic acid and water For 1:100~3:100, to increase the dissolubility of chitosan, and the viscosity and stability of chitosan is kept, chitosan is avoided to occur The phenomenon that self aggregation;It is added and keeps Fe3O4The FeCl of particle dispersing uniformity3·6H2O and FeCl2·4H2O source of iron, forming component Uniform Fe3O4/ Chitosan Composites;And pH value of solution is adjusted, heating and thermal insulation improves reaction rate, prepares high-efficiency and economic environmental protection Heavy metal chelant;Meanwhile, it is capable to which substituting crosslinking agent guarantees product Fe3O4The stability of Chitosan Composites, to control life Toxicity damage during production.And preparation process is simple, safety and environmental protection, avoids causing to damage to environment and human body, has extensive Application prospect and Practical significance.
It should be noted last that the above specific embodiment is only used to illustrate the technical scheme of the present invention and not to limit it, Although being described the invention in detail referring to example, those skilled in the art should understand that, it can be to the present invention Technical solution be modified or replaced equivalently, without departing from the spirit and scope of the technical solution of the present invention, should all cover In the scope of the claims of the present invention.

Claims (6)

1. a kind of heavy metal chelant Fe3O4The preparation method of Chitosan Composites characterized by comprising
Chitosan is dissolved in aqueous acetic acid, with obtained solution A;Wherein, the concentration range of the solution A is 1g/L~30g/ L, in the aqueous acetic acid, the range of the volume ratio of acetic acid and water is 1:100~3:100;
By FeCl3·6H2O and FeCl2·4H2O is dissolved in distilled water, with obtained solution B;Wherein, ferric ion and ferrous iron The concentration ratio of ion is 2:1, and the concentration range of the ferric ion is 0.1mol/L~1mol/L;
Alkaline solution and the solution A are sequentially added in the solution B, with obtained solution C;
The pH value of solution C is adjusted, and is heated, is kept the temperature, and resulting black product is used into deionized water and anhydrous second respectively Alcohol washing, it is dry, obtain Fe3O4Chitosan Composites.
2. heavy metal chelant Fe as described in claim 13O4The preparation method of Chitosan Composites, it is characterised in that: institute Stating alkaline solution is industrial ammonia or sodium hydrate aqueous solution.
3. heavy metal chelant Fe as described in claim 13O4The preparation method of Chitosan Composites, it is characterised in that: institute The pH value range for stating solution C is 8~10.
4. heavy metal chelant Fe as claimed in claim 33O4The preparation method of Chitosan Composites, it is characterised in that: add The temperature range of heat is 60 DEG C~80 DEG C.
5. heavy metal chelant Fe as claimed in claim 43O4The preparation method of Chitosan Composites, it is characterised in that: protect The time range of temperature is 3h~10h.
6. heavy metal chelant Fe as described in claim 13O4The preparation method of Chitosan Composites, it is characterised in that: institute State Fe3O4In Chitosan Composites, Fe3O4It than range is 1:1~1:4 with the quality of chitosan.
CN201910054492.5A 2019-01-21 2019-01-21 A kind of heavy metal chelant Fe3O4The preparation method of Chitosan Composites Pending CN109794224A (en)

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Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102134334A (en) * 2010-12-29 2011-07-27 厦门大学 Method for preparing magnetic chitosan microspheres
CN102850599A (en) * 2012-09-18 2013-01-02 厦门大学 Magnetic chitosan/nano Fe3O4 composite and preparation method and application thereof

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102134334A (en) * 2010-12-29 2011-07-27 厦门大学 Method for preparing magnetic chitosan microspheres
CN102850599A (en) * 2012-09-18 2013-01-02 厦门大学 Magnetic chitosan/nano Fe3O4 composite and preparation method and application thereof

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Application publication date: 20190524