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 PDFInfo
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- 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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- solution
- chitosan
- heavy metal
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- chitosan composites
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- 229920001661 Chitosan Polymers 0.000 title claims abstract description 50
- 239000002131 composite material Substances 0.000 title claims abstract description 32
- 229910001385 heavy metal Inorganic materials 0.000 title claims abstract description 24
- 239000013522 chelant Substances 0.000 title claims abstract description 22
- 238000002360 preparation method Methods 0.000 title claims abstract description 22
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims abstract description 51
- 239000000243 solution Substances 0.000 claims abstract description 38
- SZVJSHCCFOBDDC-UHFFFAOYSA-N iron(II,III) oxide Inorganic materials O=[Fe]O[Fe]O[Fe]=O SZVJSHCCFOBDDC-UHFFFAOYSA-N 0.000 claims abstract description 31
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 16
- VTLYFUHAOXGGBS-UHFFFAOYSA-N Fe3+ Chemical compound [Fe+3] VTLYFUHAOXGGBS-UHFFFAOYSA-N 0.000 claims abstract description 8
- 229910001447 ferric ion Inorganic materials 0.000 claims abstract description 8
- 239000012670 alkaline solution Substances 0.000 claims abstract description 7
- 229910021577 Iron(II) chloride Inorganic materials 0.000 claims abstract description 6
- NMCUIPGRVMDVDB-UHFFFAOYSA-L iron dichloride Chemical compound Cl[Fe]Cl NMCUIPGRVMDVDB-UHFFFAOYSA-L 0.000 claims abstract description 6
- 229910021578 Iron(III) chloride Inorganic materials 0.000 claims abstract description 4
- 239000008367 deionised water Substances 0.000 claims abstract description 4
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 4
- 239000012153 distilled water Substances 0.000 claims abstract description 4
- RBTARNINKXHZNM-UHFFFAOYSA-K iron trichloride Chemical compound Cl[Fe](Cl)Cl RBTARNINKXHZNM-UHFFFAOYSA-K 0.000 claims abstract description 4
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract 2
- CWYNVVGOOAEACU-UHFFFAOYSA-N Fe2+ Chemical compound [Fe+2] CWYNVVGOOAEACU-UHFFFAOYSA-N 0.000 claims abstract 2
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 14
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims description 6
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 6
- 150000002500 ions Chemical class 0.000 claims description 5
- 229910021529 ammonia Inorganic materials 0.000 claims description 3
- 239000007864 aqueous solution Substances 0.000 claims description 3
- 235000011121 sodium hydroxide Nutrition 0.000 claims description 3
- 238000005406 washing Methods 0.000 claims description 3
- 230000007613 environmental effect Effects 0.000 abstract description 9
- 238000000034 method Methods 0.000 abstract description 6
- 231100000419 toxicity Toxicity 0.000 abstract description 3
- 230000001988 toxicity Effects 0.000 abstract description 3
- 229960000935 dehydrated alcohol Drugs 0.000 abstract 1
- 229910001448 ferrous ion Inorganic materials 0.000 abstract 1
- 239000003431 cross linking reagent Substances 0.000 description 6
- 238000010438 heat treatment Methods 0.000 description 4
- 229910052742 iron Inorganic materials 0.000 description 4
- 238000004220 aggregation Methods 0.000 description 3
- 230000002776 aggregation Effects 0.000 description 3
- 238000006243 chemical reaction Methods 0.000 description 3
- 230000000694 effects Effects 0.000 description 2
- IDGUHHHQCWSQLU-UHFFFAOYSA-N ethanol;hydrate Chemical compound O.CCO IDGUHHHQCWSQLU-UHFFFAOYSA-N 0.000 description 2
- 238000009413 insulation Methods 0.000 description 2
- -1 iron ion Chemical class 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 238000004321 preservation Methods 0.000 description 2
- LRWZZZWJMFNZIK-UHFFFAOYSA-N 2-chloro-3-methyloxirane Chemical compound CC1OC1Cl LRWZZZWJMFNZIK-UHFFFAOYSA-N 0.000 description 1
- SXRSQZLOMIGNAQ-UHFFFAOYSA-N Glutaraldehyde Chemical compound O=CCCCC=O SXRSQZLOMIGNAQ-UHFFFAOYSA-N 0.000 description 1
- 206010029350 Neurotoxicity Diseases 0.000 description 1
- 206010044221 Toxic encephalopathy Diseases 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 230000000274 adsorptive effect Effects 0.000 description 1
- 238000007385 chemical modification Methods 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 231100000135 cytotoxicity Toxicity 0.000 description 1
- 230000003013 cytotoxicity Effects 0.000 description 1
- 239000000428 dust Substances 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 239000010881 fly ash Substances 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000007135 neurotoxicity Effects 0.000 description 1
- 231100000228 neurotoxicity Toxicity 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 231100000331 toxic Toxicity 0.000 description 1
- 231100000167 toxic agent Toxicity 0.000 description 1
- 230000002588 toxic effect Effects 0.000 description 1
- 239000003440 toxic substance Substances 0.000 description 1
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- Polysaccharides And Polysaccharide Derivatives (AREA)
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
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.
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Citations (2)
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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2019
- 2019-01-21 CN CN201910054492.5A patent/CN109794224A/en active Pending
Patent Citations (2)
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 |