CN106215880A - The preparation method of chitosan magnetic bead - Google Patents
The preparation method of chitosan magnetic bead Download PDFInfo
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- CN106215880A CN106215880A CN201610798725.9A CN201610798725A CN106215880A CN 106215880 A CN106215880 A CN 106215880A CN 201610798725 A CN201610798725 A CN 201610798725A CN 106215880 A CN106215880 A CN 106215880A
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- chitosan
- magnetic bead
- ethylene glycol
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- 229920001661 Chitosan Polymers 0.000 title claims abstract description 53
- 239000011324 bead Substances 0.000 title claims abstract description 27
- 238000002360 preparation method Methods 0.000 title claims abstract description 20
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims abstract description 69
- 238000003756 stirring Methods 0.000 claims abstract description 37
- 239000000243 solution Substances 0.000 claims abstract description 31
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 18
- ZNCPFRVNHGOPAG-UHFFFAOYSA-L sodium oxalate Chemical compound [Na+].[Na+].[O-]C(=O)C([O-])=O ZNCPFRVNHGOPAG-UHFFFAOYSA-L 0.000 claims abstract description 16
- 239000011259 mixed solution Substances 0.000 claims abstract description 13
- 239000000203 mixture Substances 0.000 claims abstract description 12
- 239000002244 precipitate Substances 0.000 claims abstract description 11
- 238000010438 heat treatment Methods 0.000 claims abstract description 9
- 150000002505 iron Chemical class 0.000 claims abstract description 9
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 9
- 238000001035 drying Methods 0.000 claims abstract description 3
- 238000005406 washing Methods 0.000 claims abstract description 3
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 10
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 8
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 6
- 239000007788 liquid Substances 0.000 claims description 3
- 238000002156 mixing Methods 0.000 claims description 3
- 229910021578 Iron(III) chloride Inorganic materials 0.000 claims description 2
- 239000012467 final product Substances 0.000 claims description 2
- RBTARNINKXHZNM-UHFFFAOYSA-K iron trichloride Chemical group Cl[Fe](Cl)Cl RBTARNINKXHZNM-UHFFFAOYSA-K 0.000 claims description 2
- 229910000360 iron(III) sulfate Inorganic materials 0.000 claims description 2
- 230000002459 sustained effect Effects 0.000 claims description 2
- VTLYFUHAOXGGBS-UHFFFAOYSA-N Fe3+ Chemical compound [Fe+3] VTLYFUHAOXGGBS-UHFFFAOYSA-N 0.000 claims 2
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 claims 2
- 150000003839 salts Chemical class 0.000 claims 2
- 238000006243 chemical reaction Methods 0.000 abstract description 8
- 239000002245 particle Substances 0.000 abstract description 7
- 238000000926 separation method Methods 0.000 abstract description 4
- 238000000034 method Methods 0.000 abstract description 3
- 238000004519 manufacturing process Methods 0.000 abstract description 2
- 238000001291 vacuum drying Methods 0.000 description 4
- 239000002028 Biomass Substances 0.000 description 3
- 239000003463 adsorbent Substances 0.000 description 3
- 229910001385 heavy metal Inorganic materials 0.000 description 3
- 239000000017 hydrogel Substances 0.000 description 3
- SZVJSHCCFOBDDC-UHFFFAOYSA-N iron(II,III) oxide Inorganic materials O=[Fe]O[Fe]O[Fe]=O SZVJSHCCFOBDDC-UHFFFAOYSA-N 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 230000015572 biosynthetic process Effects 0.000 description 2
- 238000009826 distribution Methods 0.000 description 2
- 229920005615 natural polymer Polymers 0.000 description 2
- 238000001179 sorption measurement Methods 0.000 description 2
- 229920002101 Chitin Polymers 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000005587 bubbling Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 150000004676 glycans Chemical class 0.000 description 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
- 239000010842 industrial wastewater Substances 0.000 description 1
- 229920002521 macromolecule Polymers 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 229920001282 polysaccharide Polymers 0.000 description 1
- 239000005017 polysaccharide Substances 0.000 description 1
- 125000002924 primary amino group Chemical group [H]N([H])* 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 230000008929 regeneration Effects 0.000 description 1
- 238000011069 regeneration method Methods 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 238000010189 synthetic method Methods 0.000 description 1
Classifications
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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
- B01J20/22—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising organic material
- B01J20/24—Naturally occurring macromolecular compounds, e.g. humic acids or their derivatives
-
- 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
-
- 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
- B01J20/28016—Particle form
- B01J20/28019—Spherical, ellipsoidal or cylindrical
Landscapes
- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Pharmaceuticals Containing Other Organic And Inorganic Compounds (AREA)
- Polysaccharides And Polysaccharide Derivatives (AREA)
- Cosmetics (AREA)
Abstract
The invention discloses the preparation method of a kind of chitosan magnetic bead, comprise the following steps: (1), by trivalent iron salt and ethylene glycol mix and blend, forms settled solution A；(2) chitosan and Disodium oxalate. are added in ethylene glycol, mix and blend, form settled solution B；(3), after step (1) gained solution A being passed through nitrogen bubble 0.5 2 hours under stirring, slowly step (2) gained solution B is added, then mixed solution is heated to 160 200 DEG C, continuously stirred reaction 12 48 hours；(4) stop stirring and heating, collect precipitate and carry out washing and be drying to obtain chitosan magnetic bead.The preparation method of the chitosan magnetic bead of the present invention has the advantage that technique is simple, convenient separation, saves the energy, is prone to industrial operation, and production security is good；Preparing gained chitosan magnetic bead uniform particle diameter, mechanical strength is good, and pattern is good.
Description
Technical field
The invention belongs to macromolecule environmentally conscious materials technical field, especially relate to the preparation side of a kind of chitosan magnetic bead
Method.
Background technology
Biomass natural polymer is considered as the removing heavy metals adsorbent of a kind of function admirable, because the natural height of biomass
Molecule is generally of the feature such as regeneration nontoxic, easy, biodegradable, environmental friendliness, wide material sources.Wherein, chitosan is exactly
The polysaccharide material of excellent properties, it derives from chitin, is the biomass natural polymer of the most second largest abundance
Son.Owing to having abundant hydroxyl and amino on chitosan molecule chain backbone, there is prominent chelating effect, can be as efficiently inhaling
Attached dose is used for removing heavy metals in industrial wastewater.Improve the adsorption capacity of chitosan class adsorbent and increase its rate of departure,
Design and develop the focus that novel chitosan class adsorbent is research at present.
Traditional way is that chitosan is made the form of hydrogel, and hydrogel is amorphous state, result of which
The ability of chitosan Adsorption of Heavy Metals can be improved to a certain extent.But the chitosan mechanical strength of hydrogel form compares
Difference, solid-liquid separation is relatively difficult.Use magnetic Nano Fe3O4Particulate load chitosan can well solve asking of solid-liquid separation
Topic, such as, have research that chitosan chain is grafted onto nano level Fe3O4Chitosan magnetic bead is made on spheroidal particle, but he
Synthetic method extremely complex, at least need three steps, i.e. Fe3O4Synthesis, surface modification and chitosan grafting.
Summary of the invention
Goal of the invention: for problems of the prior art, the invention provides a kind of easy chitosan magnetic little
The preparation method of ball.
Technical scheme: the preparation method of chitosan magnetic bead of the present invention, comprises the following steps:
(1) by trivalent iron salt and ethylene glycol mix and blend, settled solution A is formed；
(2) chitosan and Disodium oxalate. are added in ethylene glycol, mix and blend, form settled solution B；
(3) after step (1) gained solution A being passed through nitrogen bubble 0.5-2 hour under stirring, by step (2) institute
Obtain solution B to add in solution A, mixed solution is heated to 160-200 DEG C, sustained response 12-48 hour under stirring condition；
(4) stop stirring and heating, collect precipitate and carry out washing and be drying to obtain chitosan magnetic bead.
Preferably, in step (1), described trivalent iron salt is FeCl3˙6H2O、Fe2(SO4)3˙H2O and Fe (NO3)3˙9H2O
In at least one.
Preferably, in step (1), the amount ratio 1:5-10 of trivalent iron salt and ethylene glycol.
Preferably, in step (2), the amount ratio 1:1-15:5-10 of chitosan, Disodium oxalate. and ethylene glycol.
It is further preferred that in step (2), the amount ratio 1:5-10:5-10 of chitosan, Disodium oxalate. and ethylene glycol.
Preferably, in step (3), in described mixed solution, the mass ratio of trivalent iron salt, chitosan and Disodium oxalate. is 1:1-
10:2-15。
It is further preferred that in step (3), the mass ratio of trivalent iron salt, chitosan and Disodium oxalate. in described mixed solution
For 1:5-6:8-10.
Preferably, in step (1) and (2), stir speed (S.S.) is 10r/min-200r/min, and mixing time is 0.5-2h.
It is further preferred that in step (1) and (2), stir speed (S.S.) is 80-120r/min, and mixing time is 1-1.5h.
Preferably, in step (3), stir speed (S.S.) is 10r/min-200r/min, preferably 80-120r/min.
It is further preferred that in step (3), reaction temperature is 180-190 DEG C, the response time is 24-36h.
Preferably, step (4) is washed with ethanol and water after collecting precipitate respectively respectively, then does in 50-100 DEG C of vacuum
Dry 12-24h and get final product.
It is further preferred that described being dried of step (4) is vacuum dried 16-20h at 50-60 DEG C.
The chitosan magnetic bead that above-mentioned preparation method prepares is the most within the scope of the present invention.
Preparing gained chitosan magnetic bead uniform particle diameter, particle size range is 100-800nm.
Raw materials used in this preparation method it is market purchasing gained.
Beneficial effect: be compared to prior art, the preparation method of the chitosan magnetic bead of the present invention has following excellent
Point: (1) technique is simple, convenient separation, saves the energy, is prone to industrial operation, and production security is good；(2) gained magnetic is prepared
Chitosan Beads uniform particle diameter, particle diameter is 100-800nm；Pattern is good.
Accompanying drawing explanation
Fig. 1 is the Electronic Speculum figure preparing gained chitosan magnetic bead；
Fig. 2 is the DLS grain size distribution preparing gained chitosan magnetic bead.
Detailed description of the invention
Embodiment 1
5.4g FeCl is put in reactor 13˙6H2O and 54ml ethylene glycol, is formed after stirring 2h with the speed of 10r/min
Settled solution A；In reactor 2, put into 5.4g chitosan and 27g Disodium oxalate., be dissolved in 54ml ethylene glycol, with 50r/min's
Settled solution B is formed after speed stirring 1.5h；The stir speed (S.S.) of 100r/min opened by reactor 1, is passed through nitrogen bubble 0.5 hour
After, the settled solution B in reactor 2 is poured in reactor 1 slowly, mixed solution in reactor 1 is heated to 160 DEG C,
Continuously stirred reaction 48 hours；Stop stirring and heating, precipitate second alcohol and water is cleaned, dry in 50 DEG C of vacuum drying ovens
Dry 24h, obtains chitosan magnetic bead.
Embodiment 2
5.4g FeCl is put in reactor 13˙6H2O and 43.2ml ethylene glycol, stirs 0.5h with the speed of 200r/min
Rear formation settled solution A；In reactor 2, put into 27g chitosan and 54g Disodium oxalate., be dissolved in 216ml ethylene glycol, with
Settled solution B is formed after the speed stirring 1.5h of 50r/min；The stir speed (S.S.) of 10r/min opened by reactor 1, is passed through nitrogen drum
After steeping 2 hours, the settled solution B in reactor 2 is poured in reactor 1 slowly, mixed solution in reactor 1 is heated to
185 DEG C, continuously stirred reaction 36 hours；Stop stirring and heating, precipitate second alcohol and water is cleaned, does in 100 DEG C of vacuum
Dry case is dried 12h, obtains chitosan magnetic bead.
Embodiment 3
8.0g Fe is put in reactor 12(SO4)3˙H2O and 40ml ethylene glycol, after stirring 2h with the speed of 150r/min
Form settled solution A；In reactor 2, put into 32g chitosan and 40g Disodium oxalate., be dissolved in 160ml ethylene glycol, with 150r/
Settled solution B is formed after the speed stirring 2h of min；The stir speed (S.S.) of 200r/min opened by reactor 1, is passed through nitrogen bubble 2 little
Shi Hou, pours in reactor 1 by the settled solution B in reactor 2 slowly, and mixed solution in reactor 1 is heated to 200
DEG C, continuously stirred reaction 24 hours；Stop stirring and heating, precipitate second alcohol and water is cleaned, at 80 DEG C of vacuum drying ovens
In be dried 18h, obtain chitosan magnetic bead.
Embodiment 4
8.0g Fe is put in reactor 12(SO4)3˙H2O and 64ml ethylene glycol, after stirring 1h with the speed of 120r/min
Form settled solution A；In reactor 2, put into 80g chitosan and 120g Disodium oxalate., be dissolved in 400ml ethylene glycol, with
Settled solution B is formed after the speed stirring 1h of 120r/min；The stir speed (S.S.) of 120r/min opened by reactor 1, is passed through nitrogen drum
After steeping 2 hours, the settled solution B in reactor 2 is poured in reactor 1 slowly, mixed solution in reactor 1 is heated to
190 DEG C, continuously stirred reaction 12 hours；Stop stirring and heating, precipitate second alcohol and water is cleaned, 50 DEG C of vacuum drying
Case is dried 24h, obtains chitosan magnetic bead.
Embodiment 5
8.1g Fe (NO is put in reactor 13)39H2O and 81ml ethylene glycol, after stirring 1.5h with the speed of 80r/min
Form settled solution A；In reactor 2, put into 8.1g chitosan and 16.2g Disodium oxalate., be dissolved in 40.5ml ethylene glycol, with
Settled solution B is formed after the speed stirring 1.5h of 80r/min；The stir speed (S.S.) of 80r/min opened by reactor 1, is passed through nitrogen drum
After steeping 0.5 hour, the settled solution B in reactor 2 is poured in reactor 1 slowly, mixed solution in reactor 1 is heated
To 160 DEG C, continuously stirred reaction 48 hours；Stop stirring and heating, precipitate second alcohol and water is cleaned, does in 60 DEG C of vacuum
Dry case is dried 20h, obtains chitosan magnetic bead.
Embodiment 6
8.1g Fe (NO is put in reactor 13)39H2O and 64.8ml ethylene glycol, stirs 1.5h with the speed of 10r/min
Rear formation settled solution A；In reactor 2, put into 32.4g chitosan and 40.4g Disodium oxalate., be dissolved in 324ml ethylene glycol,
Settled solution B is formed after stirring 1.5h with the speed of 10r/min；The stir speed (S.S.) of 120r/min opened by reactor 1, is passed through nitrogen
After bubbling 2 hours, the settled solution B in reactor 2 is poured in reactor 1 slowly, mixed solution in reactor 1 is heated
To 200 DEG C, continuously stirred reaction 24 hours；Stop stirring and heating, precipitate second alcohol and water is cleaned, in 100 DEG C of vacuum
Drying baker is dried 15h, obtains chitosan magnetic bead.
Example 1-6 prepares gained chitosan magnetic bead and carries out DLS analysis, and Fig. 2 is shown in the distribution of gained DLS particle diameter, number
Calculating average result such as table 1 the most afterwards:
The DLS of table 1 chitosan magnetic bead analyzes
Claims (10)
1. the preparation method of a chitosan magnetic bead, it is characterised in that comprise the following steps:
(1) by trivalent iron salt and ethylene glycol mix and blend, settled solution A is formed；
(2) chitosan and Disodium oxalate. are added in ethylene glycol, mix and blend, form settled solution B；
(3) after step (1) gained solution A being passed through nitrogen bubble 0.5-2 hour under stirring, by molten for step (2) gained
Liquid B adds in solution A, mixed solution is heated to 160-200 DEG C, sustained response 12-48 hour under stirring condition；
(4) stop stirring and heating, collect precipitate and carry out washing and be drying to obtain chitosan magnetic bead.
Preparation method the most according to claim 1, it is characterised in that in step (1), described trivalent iron salt is FeCl3˙
6H2O、Fe2(SO4)3˙H2O and Fe (NO3)3˙9H2At least one in O.
Preparation method the most according to claim 1, it is characterised in that in step (1), trivalent iron salt and the consumption of ethylene glycol
Compare 1:5-10.
Preparation method the most according to claim 1, it is characterised in that in step (2), chitosan, Disodium oxalate. and ethylene glycol
Amount ratio 1:2-15:5-10.
Preparation method the most according to claim 1, it is characterised in that in step (3), ferric iron in described mixed solution
The mass ratio of salt, chitosan and Disodium oxalate. is 1:1-10:2-15.
Preparation method the most according to claim 5, it is characterised in that in step (3), ferric iron in described mixed solution
The mass ratio of salt, chitosan and Disodium oxalate. is 1:5-6:8-10.
Preparation method the most according to claim 1, it is characterised in that in step (1) and (2), stir speed (S.S.) is 10r/
Min-200r/min, mixing time is 0.5-2h.
Preparation method the most according to claim 1, it is characterised in that in step (3), stir speed (S.S.) is 10r/min-
200r/min。
Preparation method the most according to claim 1, it is characterised in that step (4) collect after precipitate respectively with ethanol and
Water washs, and is then vacuum dried 12-24h at 50-100 DEG C and get final product.
10. the chitosan magnetic bead that in claim 1～9, any one preparation method prepares.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610798725.9A CN106215880A (en) | 2016-08-31 | 2016-08-31 | The preparation method of chitosan magnetic bead |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610798725.9A CN106215880A (en) | 2016-08-31 | 2016-08-31 | The preparation method of chitosan magnetic bead |
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ID=58074141
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109876779A (en) * | 2019-01-28 | 2019-06-14 | 湖南城市学院 | A kind of mesoporous nano Fe3O4The preparation and application of chitosan core-shell crosslinked microsphere material |
| CN110075810A (en) * | 2019-01-31 | 2019-08-02 | 中冶华天南京工程技术有限公司 | Polystyrene-based chitosan magnetic core-shell composite material and preparation method |
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| CN105618005A (en) * | 2016-03-29 | 2016-06-01 | 山西大学 | Preparation method of magnetic chitosan |
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2016
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103041777A (en) * | 2013-01-28 | 2013-04-17 | 天津市水利科学研究院 | Fe3O4/CS magnetic material adsorbent, preparation method of Fe3O4/CS magnetic material adsorbent, and sewage treatment method |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109876779A (en) * | 2019-01-28 | 2019-06-14 | 湖南城市学院 | A kind of mesoporous nano Fe3O4The preparation and application of chitosan core-shell crosslinked microsphere material |
| CN109876779B (en) * | 2019-01-28 | 2022-09-13 | 湖南城市学院 | Nano mesoporous Fe 3 O 4 Preparation and application of-chitosan core-shell crosslinked microsphere material |
| CN110075810A (en) * | 2019-01-31 | 2019-08-02 | 中冶华天南京工程技术有限公司 | Polystyrene-based chitosan magnetic core-shell composite material and preparation method |
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