CN108722360A - A kind of preparation method of recombination chitosan - Google Patents
A kind of preparation method of recombination chitosan Download PDFInfo
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- CN108722360A CN108722360A CN201810071191.9A CN201810071191A CN108722360A CN 108722360 A CN108722360 A CN 108722360A CN 201810071191 A CN201810071191 A CN 201810071191A CN 108722360 A CN108722360 A CN 108722360A
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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
- B01J20/048—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 containing phosphorus, e.g. phosphates, apatites, hydroxyapatites
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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
- B01J20/06—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising oxides or hydroxides of metals not provided for in group B01J20/04
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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
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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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- 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
- B01J20/28021—Hollow particles, e.g. hollow spheres, microspheres or cenospheres
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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- B01J2220/00—Aspects relating to sorbent materials
- B01J2220/40—Aspects relating to the composition of sorbent or filter aid materials
- B01J2220/46—Materials comprising a mixture of inorganic and organic materials
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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
- B01J2220/00—Aspects relating to sorbent materials
- B01J2220/40—Aspects relating to the composition of sorbent or filter aid materials
- B01J2220/48—Sorbents characterised by the starting material used for their preparation
- B01J2220/4806—Sorbents characterised by the starting material used for their preparation the starting material being of inorganic character
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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
- B01J2220/00—Aspects relating to sorbent materials
- B01J2220/40—Aspects relating to the composition of sorbent or filter aid materials
- B01J2220/48—Sorbents characterised by the starting material used for their preparation
- B01J2220/4812—Sorbents characterised by the starting material used for their preparation the starting material being of organic character
- B01J2220/4825—Polysaccharides or cellulose materials, e.g. starch, chitin, sawdust, wood, straw, cotton
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Abstract
The invention discloses a kind of preparation methods of recombination chitosan, it is characterised in that：Ferroso-ferric oxide is prepared in advance, then it carries out ionomer with CTS/HTCC with sodium polyphosphate (TPP) to react (precrosslink), glutaraldehyde (25%) is reacted with the amino on CTS/HTCC generates Schiff (RN=CH2) it is full cross-linked formed with some strength sphere, by a certain amount of CTS/HTCC and appropriate pore-foaming agent polyethylene glycol stirring and dissolving in 2% acetums of 40ml, be added Fe3O4, stir and add ultrasound 20min, 100ml atoleines and a certain amount of Span80 are added in three-necked flask, 240rpm stirs 40min at 40 DEG C, rotating speed is improved to 360rpm, is sufficiently stirred 60min, forms uniform lotion, then certain density TPP dopes are added and carry out precrosslink, after being sufficiently stirred 30min, glutaraldehyde (25%), 40 degree of isothermal reaction 5h are added, it centrifuges, is washed repeatedly 5 times with absolute ethyl alcohol and deionized water.Its advantage is that：Adsorption effect is good, and manufacturing cost is low.
Description
Technical field
The present invention relates to a kind of preparation method fields of recombination chitosan, and in particular to a kind of system of magnetic coupling chitosan
Preparation Method.
Background technology
Water resource pollution and shortage oneself through seriously affecting expanding economy and social productive forces, also limit people's lives water
Flat raising, therefore, sewage disposal technology also receive extensive concern both domestic and external.For current Water Pollution Problem, scientific research work
Author proposes many method for treating water, such as absorption, coagulation, ion exchange and membrane filtration.Wherein, absorption method is because of its design and operation
Simply, investment cost is low, easily operated, all has many advantages, such as higher adsorption efficiency to multiple pollutant, it is considered to be a kind of
Effective method for treating water.
Absorption method is a kind of method by adding adsorbent into water by pollutant removal.Absorption method is not only to humic acid
Equal organic matters have higher removal efficiency, also can remove heavy metal ion and each pollutant in water, are now subjected to wide
The attention of big water treatment work person.
Chitosan is the alkaline carbohydrate natural polymer uniquely found in current nature.Not soluble in water and aqueous slkali, can
It is dissolved in most of organic acid and glacial acetic acid.Contain-OH ,-NHCOCH in chitosan molecule structure3, free state amino and hydroxyl
It is highly active.In addition, chitosan has the unique properties such as biological degradability, cellular affinity and biological effect, thus
The recombination chitosan of invention, has chitosan intrinsic propesties and magnetism, thus with good film forming, adsorptivity, fibre forming property,
Moisture retention and antibiotic property etc..
Free amine group easily combines H under mild acid conditions in chitosan molecule+So that chitosan carries part positive charge, energy
With in solution suspend and electronegative particle assembled by electrostatic interaction, or formed complex compound and flocculate.Chitosan
The bonding effect of macromolecular chain can and organic molecule, such as phenolic compound, quinones combine form covalent bond, hydrogen bond,
Chemisorption occurs.Therefore adsorbent, the flocculant being widely used as in water process.Further, since in molecule there are hydroxyl,
Amino and other groups, chitosan can borrow hydrogen bond to form the cage molecule with similar reticular structure, can be with many metal ions
It is chelated, therefore effectively the heavy metal ion in adsorbent solution can form chelating body.But due to only in acid condition
Show electropositive, therefore pH application ranges are relatively narrow, its electropositive can be greatly improved by quaternization, and then make chitosan season
Ammonium salt derivatives are also widely applied in water process.
But the non-porous laminated structure of chitosan, cause its specific surface area smaller, and soluble loss under acid condition, makes
Its adsorption efficiency is relatively low, separation property is poor.Powdered chitosan grain size is small, and adsorbent is caused to detach difficulty with solution.And shell
Glycan only can just show the property of Polycationic electrolyte after protonated amino under mildly acidic conditions, and lotus positive electricity ability by
PH is affected, therefore we need to find a kind of adsorbent that can solve the above technical problem.
Invention content
The purpose of the present invention is to solve the above technical problem, provide that a kind of adsorption effect is good, can be easily separated, has one
Fixed cavernous structure, the lower recombination chitosan preparation method of manufacturing cost.
The technical scheme is that such：A kind of preparation method of magnetic coupling chitosan, it is characterised in that：
Step 1：Weigh 7.82gFecl3.6H2O and 3.61Fecl2.4H2O is dissolved in 150ml deionized waters,
It is placed in 250mL three-necked flasks, in N2Under protection, it is slowly added to controlled at 40 DEG C by heating water bath mechanical agitation
38mLNH3.H2O (25% concentration), is stirred continuously 30min, then heats to 65 DEG C, and two hours are kept under constant temperature, can be obtained
Black suspension is detached by magnet after cooling, is washed with distilled water arrives neutrality for several times later, 50 DEG C of vacuum drying
12h, you can obtain required magnetic ferroferric oxide, take the sample to be ground spare.
Step 2：It is initially formed water-in-oil emulsion structure, ionomer is carried out with sodium polyphosphate (TPP) and CTS/HTCC
It reacts (precrosslink), forms preliminary cation crosslinking nano grade microballoon；Then, glutaraldehyde reacts generation with the amino on CTS/HTCC
Schiff (RN=CH2) it is full cross-linked formed with some strength sphere；By a certain amount of CTS/HTCC and appropriate pore
Agent polyethylene glycol PEG2000 stirring and dissolvings, according to certain mol ratio, are added step 1 and prepare in 2% acetums of 40ml
Ferroso-ferric oxide；Ultrasonic 20min is allowed to be dispersed in the above solution, and 100ml atoleines are added in three-necked flask
With a certain amount of Span80；At 65 DEG C, 240rpm stirs 40min, mixes well and is configured to oil phase.The configured water phase by before
Solution adds in oil phase dropwise, and rotating speed is improved to 360rpm, is sufficiently stirred 60min, forms uniform lotion；Then it is added certain dense
The TPP dopes of degree carry out precrosslink, after being sufficiently stirred 30min, are added glutaraldehyde (25%), 65 DEG C of isothermal reaction 5h, then from
The heart detaches, and is washed repeatedly 5 times with absolute ethyl alcohol and deionized water, keeps in deionized water.
Preferably, the recombination chitosan is in unifonn spherical, and average grain diameter is in 1~2mm.-
Preferably, CTS/HTCC ratios 1: 1 in described experiment, TPP usage amounts 17%.
Adsorption mechanism is tested：The methyl orange solution of a concentration of 50mg/L of 300ml is taken to be added in conical flask, weight in wet base, which is added, is
0.3 CHMMs (preparation condition CTS/HTCC=I: 1, TPP5%=17%), at room temperature with the rotating speed constant temperature oscillation of 200rpm
It is measured by sampling after 2h, calculates its equilibrium adsorption capacity.Adsorbent after absorption is taken out, with 1mol/L NaCl and 0.1mol/L
Into Mobile state regeneration treatment NaCl and the NaOH residual of attachment removal is washed with deionized water, then again in NaOH mixed solutions after regeneration
Secondary addition 300ml methyl orange solutions continue at room temperature to be measured by sampling after the rotating speed isothermal vibration 2h of 200rpm and calculate it
Adsorbance repeats above operation 6 times.
Beneficial effects of the present invention：
1, using inverse suspension crosslinking method, using sodium polyphosphate TPP as precrosslinker, glutaraldehyde as rear crosslinking agents,
Prepare recombination chitosan magnetic microsphere.The composite crosslinking mode that this method is combined using ionomer and chemical covalent cross-linked phase,
Microballoon obtained has higher mechanical strength.
2, recombination chitosan has ion exchange and physical absorption ability, can significantly improve to natural organic matter, methyl orange
Etc. the electrical organic matter of bears removal effect.
3. the recombination chitosan prepared by the present invention is at low cost, convenient for separation.
Description of the drawings
Fig. 1 is magnetic coupling chitosan preparation facilities figure of the present invention.
Fig. 2 is different TPP dosages magnetic recombination chitosan grain size distributions.
Specific implementation mode
As shown in Fig. 1 to 2, the present invention is such to work, illustrates in conjunction with the accompanying drawings and embodiments, and a kind of Composite Shell is poly-
The preparation method of sugar, it is characterised in that：
Step 1：Weigh 7.82gFecl3.6H2O and 3.61Fecl2.4H2O is dissolved in 150ml deionized waters,
It is placed in 250mL three-necked flasks, in N2Under protection, it is slowly added to controlled at 40 DEG C by heating water bath mechanical agitation
38mLNH3.H2O (25% concentration), is stirred continuously 30min, then heats to 65 DEG C, and two hours are kept under constant temperature, can be obtained
Black suspension is detached by magnet after cooling, is washed with distilled water arrives neutrality for several times later, 50 DEG C of vacuum drying
12h, you can obtain required magnetic ferroferric oxide, take the sample to be ground spare.
Step 2：It is initially formed water-in-oil emulsion structure, ionomer is carried out with sodium polyphosphate (TPP) and CTS/HTCC
It reacts (precrosslink), forms preliminary cation crosslinking nano grade microballoon；Then, glutaraldehyde reacts generation with the amino on CTS/HTCC
Schiff (RN=CH2) it is full cross-linked formed with some strength sphere；By a certain amount of CTS/HTCC and appropriate pore
Agent polyethylene glycol PEG2000 stirring and dissolvings, according to certain mol ratio, are added step 1 and prepare in 2% acetums of 40ml
Ferroso-ferric oxide；Ultrasonic 20min is allowed to be dispersed in the above solution, and 100ml atoleines are added in three-necked flask
With a certain amount of Span80；At 65 DEG C, 240rpm stirs 40min, mixes well and is configured to oil phase.The configured water phase by before
Solution adds in oil phase dropwise, and rotating speed is improved to 360rpm, is sufficiently stirred 60min, forms uniform lotion；Then it is added certain dense
The TPP dopes of degree carry out precrosslink, after being sufficiently stirred 30min, are added glutaraldehyde (25%), 65 DEG C of isothermal reaction 5h, then from
The heart detaches, and is washed repeatedly 5 times with absolute ethyl alcohol and deionized water, keeps in deionized water.
Embodiment one：In order to study TPP dosages, to recombination chitosan, (CHMMs adsorbs the influence of humic acid, in temperature
It is 1: 1 with CTS/HTCC ratios when 293K, and TPP adds ratio condition different (on the basis of CTS and HTCC gross masses)
The recombination chitosan (CHMMs) of lower preparation adsorbs humic acid, compared with the complex microsphere for not adding sodium polyphosphate, throws
Add the recombination chitosan (CHMMs) that 17% TPP is prepared to humic acid eliminating rate of absorption, hence it is evident that be improved, absorption is held
Amount is increased to 1.74mg/g by 1.70mg/g.This is because the addition of TPP, can change the mechanical strength and particle diameter distribution of microballoon,
Substantially reduce the particle diameter distribution of composite magnetic microballoon.The ion for the complex microsphere that adsorption capacity is calculated with chapter 3 in experiment
Some gaps of exchange capacity, this also indicates that complex microsphere is not only ion exchange to the absorption of humic acid, and there are still surface objects
Manage suction-operated, and physical absorption effect is then related to the specific surface area of adsorbent, and specific surface area depends mainly on the size of
The grain size and porosity of adsorbent.Therefore, after the grain size of complex microsphere reduces, specific surface area also accordingly increases, to humic acid
Adsorption rate also get a promotion.
Claims (4)
1. a kind of preparation method of recombination chitosan, it is characterised in that：
2. step 1：Weigh 7.82gFecl3.6H2O and 3.61Fecl2.4H2O is dissolved in 150ml deionized waters, is placed in
In 250mL three-necked flasks, in N2Under protection, it is slowly added to controlled at 40 DEG C by heating water bath mechanical agitation
38mLNH3.H2O (25% concentration), is stirred continuously 30min, then heats to 65 DEG C, and two hours are kept under constant temperature, can be obtained
Black suspension is detached by magnet after cooling, is washed with distilled water arrives neutrality for several times later, 50 DEG C of vacuum drying
12h, you can obtain required magnetic ferroferric oxide, take the sample to be ground spare.Step 2：It is initially formed Water-In-Oil
Emulsion structure carries out ionomer with CTS/HTCC with sodium polyphosphate (TPP) and reacts (precrosslink), forms preliminary cation crosslinking
Nanoscale microballoon；Then, glutaraldehyde is reacted with the amino on CTS/HTCC generates Schiff (RN=CH2) full cross-linked formation
Sphere with some strength；By a certain amount of CTS/HTCC and appropriate pore-foaming agent polyethylene glycol PEG2000 stirring and dissolvings in
In 2% acetums of 40ml, according to certain mol ratio, ferroso-ferric oxide prepared by step 1 is added；Ultrasonic 20min, is allowed to
It is dispersed in the above solution, 100ml atoleines and a certain amount of Span80 is added in three-necked flask；At 65 DEG C,
240rpm stirs 40min, mixes well and is configured to oil phase.It configured aqueous phase solution will add to dropwise in oil phase before, rotating speed carries
Up to 360rpm is sufficiently stirred 60min, forms uniform lotion；Then certain density TPP dopes are added and carry out precrosslink, fill
After dividing stirring 30min, glutaraldehyde (25%) is added, 65 DEG C of isothermal reaction 5h are then centrifuged for detaching, with absolute ethyl alcohol and deionization
Water washs 5 times repeatedly, keeps in deionized water.
3. according to a kind of preparation method of recombination chitosan described in claim 1, it is characterised in that：Recombination chitosan is in equal
Even spherical, average grain diameter is in 1~2mm.
4. according to a kind of preparation method of recombination chitosan described in claim 1, it is characterised in that：In described experiment
CTS/HTCC ratios 1: 1, TPP usage amounts 17%.
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| CN201810071191.9A CN108722360A (en) | 2018-01-23 | 2018-01-23 | A kind of preparation method of recombination chitosan |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112275260A (en) * | 2020-07-13 | 2021-01-29 | 广西科技大学 | Chitosan/fibroin-based dual-structure porous adsorption filter material with polyethylene glycol as pore-foaming agent and preparation method thereof |
| CN114130367A (en) * | 2021-11-29 | 2022-03-04 | 北京师范大学 | Magnetic adsorption material for cleaning and decontaminating radioactive contaminated soil |
| CN114617139A (en) * | 2022-04-18 | 2022-06-14 | 永康市第一人民医院 | Spray for persistent disinfection for ICU and preparation thereof |
-
2018
- 2018-01-23 CN CN201810071191.9A patent/CN108722360A/en active Pending
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112275260A (en) * | 2020-07-13 | 2021-01-29 | 广西科技大学 | Chitosan/fibroin-based dual-structure porous adsorption filter material with polyethylene glycol as pore-foaming agent and preparation method thereof |
| CN114130367A (en) * | 2021-11-29 | 2022-03-04 | 北京师范大学 | Magnetic adsorption material for cleaning and decontaminating radioactive contaminated soil |
| CN114617139A (en) * | 2022-04-18 | 2022-06-14 | 永康市第一人民医院 | Spray for persistent disinfection for ICU and preparation thereof |
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Application publication date: 20181102 |