CN110115979A - A kind of preparation method of ferro manganese composite oxides dipping chitosan beads adsorbent - Google Patents
A kind of preparation method of ferro manganese composite oxides dipping chitosan beads adsorbent Download PDFInfo
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- CN110115979A CN110115979A CN201910161353.2A CN201910161353A CN110115979A CN 110115979 A CN110115979 A CN 110115979A CN 201910161353 A CN201910161353 A CN 201910161353A CN 110115979 A CN110115979 A CN 110115979A
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- 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
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- 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
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- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
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- B01J20/30—Processes for preparing, regenerating, or reactivating
- B01J20/32—Impregnating or coating ; Solid sorbent compositions obtained from processes involving impregnating or coating
- B01J20/3202—Impregnating or coating ; Solid sorbent compositions obtained from processes involving impregnating or coating characterised by the carrier, support or substrate used for impregnation or coating
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Abstract
The invention discloses a kind of preparation methods of ferro manganese composite oxides dipping chitosan beads adsorbent, mainly comprise the steps that step 1: by KMnO4Solution with etc. quality FeSO4Solution mixing, under nitrogen atmosphere heating reaction, centrifugation removal supernatant are dried in vacuo after washing repeatedly, roast, grind after cooling；Step 2: taking oxalic acid solution to mix with acetic acid solution, rapid freezing after the higher-order of oscillation, centrifuging and taking supernatant, and lactic acid solution is added dropwise, cooling after water-bath；Step 3: chitosan is mixed with modifier solution, using electrostatic spinning technique blending and modifying, after collecting condensing soln, distilled water is added and stirs evenly；Step 4: ferro manganese composite oxides are mixed with modification of chitosan solution, NaOH solution high speed are sprayed into mixed solution, reaction under high pressure, are collected precipitating and are dried in vacuo afterwards wash with distilled water.
Description
Technical field
The invention belongs to technical field of new material preparation, are specifically related to a kind of ferro manganese composite oxides dipping chitosan
The preparation method of pearl adsorbent.
Background technique
Claim infusion process and purpose Catalyst raw to impregnate the method for manufacturing catalyst for crucial and specific step
A kind of widely applied method in production.Infusion process is based on active component (containing co-catalyst), and dipping column are more in the form of salting liquid
On the carrier of hole and column inner surface is permeated, and forms the principle of effective catalyst.Usually go leaching each the liquid containing active material
Class carrier removes remaining liq after impregnating balance, then after carrying out the processes such as drying identical with the precipitation method, roasting, activation
Processing.Through drying, moisture is evaporated and is escaped, the salt of active component can be made to be retained on the inner surface of carrier, these metals and
The salt of metal oxide is evenly distributed in the pore of carrier, to get the carrier of high degree of dispersion after heated decomposition and activation
Catalyst.
Living solution must be immersed on carrier, and common porous carrier has aluminium oxide, silica, active carbon, silicic acid
Aluminium, diatomite, float stone, asbestos, clay, magnesia, atlapulgite etc. can use powdery, can also use particle after molding
Shape.Aluminium oxide and silica these oxide carriers have most of active carbons of absorption property the same, very with regard to image surface
It is easy to be soaked by aqueous solution.In addition, capillary force can ensure that liquid is inhaled people into entire porous structure or even one end
Closed capillary will be also filled, and the dissolution of gas in a liquid then facilitates the progress of process.But also some carriers are difficult
In soaking, such as high-graphitized or not chemically adsorbing oxygen carbon is exactly in this way, can evacuate with organic molten benefit or by carrier
Lower dipping.
Studies have shown that ferro manganese composite oxides can efficiently remove arsenic and phosphorus in water body, as it is a kind of it is nontoxic, can biology
The high molecular material of degradation, chitosan are also effective adhesive, so, ferro manganese composite oxides are coated on chitosan bone
In frame, granulated sorbent is made, can in water body arsenic and phosphorus effectively remove, still, traditional preparation method at present
Ferro manganese composite oxides obtained/chitosan intensity is inadequate, and specific surface area is small, inadequate to the removal rate of arsenic in water body and phosphorus
Height, so, design the preparation method of ferro manganese composite oxides dipping chitosan beads adsorbent a kind of very it is necessary to.
Summary of the invention
In view of the above problems, the present invention provides a kind of ferro manganese composite oxides to impregnate chitosan beads adsorbent
Preparation method.
The technical scheme is that a kind of preparation method of ferro manganese composite oxides dipping chitosan beads adsorbent, main
Want the following steps are included:
Step 1: ferro manganese composite oxides preparation
Under conditions of magnetic agitation, by KMnO4Sufficiently melt in deionized water to KMnO4Concentration is 0.3mol/L,
By KMnO4Solution is down in reaction kettle, and control reactor temperature is 20-30 DEG C, under the conditions of magnetic agitation, to reaction kettle
Interior dropwise addition and KMnO430% concentration FeSO of the quality such as solution4Solution after being added dropwise, closes reaction kettle, under nitrogen atmosphere
Heated solution reacts 1-2h to 110-120 DEG C, and it is 6.5-7.5 that pH value of solution is adjusted after standing to room temperature, is centrifuged removal supernatant,
It is dried in vacuo 18-20h at 60-70 DEG C after washing repeatedly, the precipitating after drying is placed in Muffle furnace, controls Muffle furnace temperature
Degree reaches 600 DEG C, roasts 3-4h, is ground to 60-80 mesh after cooling, obtains ferro manganese composite oxides；
Step 2: modifying agent preparation
Take the oxalic acid solution of 1mol/L to mix with the acetic acid solution of 1mol/L with the mass ratio of 1:3, at room temperature with
The hunting of frequency 15min of 10kHz, rapid freezing to 3-5 DEG C, centrifuging and taking supernatant are added dropwise and supernatant quality into supernatant
Than the 0.3mol/L lactic acid solution for 5:1, water-bath 15min in boiling water, it is cooling after up to modifier solution；
Step 3: chitin modified
Modifier solution obtained in chitosan and step 2 is uniformly mixed with the ratio of 2:1 and obtains mixed solution, it will
Mixed solution is sprayed in strong electrical field using electrostatic spinning technique carries out blending and modifying, and modified solution is collected through condenser,
It is warming up to 15-20 DEG C while distilled water is added, continues stirring until and is uniformly mixed up to modification of chitosan solution；
Step 4: ferro manganese composite oxides impregnate chitosan beads
By modification of chitosan solution obtained in ferro manganese composite oxides obtained in step 1 and step 3 with mass ratio
The ratio of 2:3 is mixed to high-pressure bottle, and the NaOH solution of 0.2mol/L is heated to 45-50 DEG C through high-pressure pump and heat exchanger
Afterwards, it is sprayed into the mixed solution in high-pressure bottle with the speed of 30-40m/s, adjusting pressure in high-pressure bottle is 50MPa reaction
3h collects depositing particles by the filter of high-pressure bottle bottom, and vacuum drying is after being cleaned repeatedly with distilled water to get ferrimanganic
Composite oxides impregnate chitosan beads adsorbent.
Further, the KMnO4For any one the common potassium permanganate that can be bought on the market, material is easy to get, raw
It produces at low cost.
Further, the washing repeatedly in the step 1 is alternately washed using dehydrated alcohol and deionized water, is washed
Wash that effect is good, and alternately washing can increase the settling property of ferro manganese composite oxides.
Further, the heating rate control of Muffle furnace is 2 DEG C/min in the step 1, makes ferrimanganic in temperature-rise period
Composite oxides undergo low-temperature prewarming to high-temperature roasting, and direct high-temperature roasting can reduce the performance of ferro manganese composite oxides.
Further, the specific steps of electrostatic spinning blending and modifying are carried out in the step 3 are as follows: by mixed solution close
It closes pressurization in container to spray through 0.5mm spray head, strong electrical field is set around spray head, ejected in forceful electric power field action knit stitch head mixed
Closing solution will form taper filamentous, and filamentous is collected through condenser plus distilled water heating fusing, electrostatic spinning blending and modifying obtain
The chitosan solution closeness arrived is high and performance is more preferable.
Further, the filter pore size of the high-pressure bottle bottom is 3.5-4.0mm, hygrometric state ferro manganese composite oxides
Chitosan beads size controlling is impregnated in 3.5-4.0mm, and it is 2.0- that dry state ferro manganese composite oxides, which impregnate chitosan beads partial size,
2.5.。
Further, in step 4 to ferro manganese composite oxides dipping chitosan beads adsorbent magnetize, can
Magnetic ferro manganese composite oxides dipping chitosan beads adsorbent is obtained, the ferro manganese composite oxides after magnetizing impregnate chitosan beads
There is good adsorptivity compared to common ferro manganese composite oxides dipping chitosan beads.
Compared with prior art, the beneficial effects of the present invention are:
(1) present invention improves traditional ferro manganese composite oxides preparation method, obtained ferro manganese composite oxides tool
There is higher mechanical strength；
(2) present invention is modified by modifying agent and chitosan blend, and chitosan is made to have the bonding force and packet of more strength
The property covered, the ferro manganese composite oxides dipping chitosan beads being prepared have biggish specific surface area and porosity；
(3) ferro manganese composite oxides are impregnated into chitosan beads under hyperbaric environment, improves the packet of ferro manganese composite oxides
Cover rate；
(4) it by ferro manganese composite oxides dipping chitosan beads adsorbent magnetization, is soaked compared to common ferro manganese composite oxides
Stain chitosan beads have good adsorptivity.
Specific embodiment
It is further to the present invention combined with specific embodiments below to be solved for convenient for the understanding to technical solution of the present invention
Explanation is released, embodiment does not constitute the restriction to invention protection scope.
Embodiment 1
A kind of preparation method of ferro manganese composite oxides dipping chitosan beads adsorbent, mainly comprises the steps that
Step 1: ferro manganese composite oxides preparation
Under conditions of magnetic agitation, the KMnO that will arbitrarily buy on the market4Sufficiently melt in deionized water to KMnO4
Concentration is 0.3mol/L, by KMnO4Solution is down in reaction kettle, and control reactor temperature is 20 DEG C, in magnetic agitation condition
Under, dropwise addition and KMnO into reaction kettle430% concentration FeSO of the quality such as solution4Solution after being added dropwise, closes reaction kettle,
Heated solution reacts 1h to 110 DEG C under nitrogen atmosphere, and it is 6.5 that pH value of solution is adjusted after standing to room temperature, centrifugation removal supernatant
Liquid is dried in vacuo 18h at 60 DEG C using after dehydrated alcohol and the washing of deionized water alternate repetition, the precipitating after drying is set
In Muffle furnace, the control of Muffle furnace heating rate makes temperature reach 600 DEG C in 2 DEG C/min, roasts 3h, is ground to 60 after cooling
Mesh obtains ferro manganese composite oxides；
Step 2: modifying agent preparation
Take the oxalic acid solution of 1mol/L to mix with the acetic acid solution of 1mol/L with the mass ratio of 1:3, at room temperature with
The hunting of frequency 15min of 10kHz, rapid freezing to 3 DEG C, centrifuging and taking supernatant are added dropwise and supernatant mass ratio into supernatant
For the 0.3mol/L lactic acid solution of 5:1, water-bath 15min in boiling water, it is cooling after up to modifier solution；
Step 3: chitin modified
Modifier solution obtained in chitosan and step 2 is uniformly mixed with the ratio of 2:1 and obtains mixed solution, it will
Mixed solution pressurizes in closed container to be sprayed through 0.5mm spray head, and strong electrical field is arranged around spray head, in forceful electric power field action knit stitch
The mixed solution that head ejects will form taper filamentous, and modified solution is collected through condenser, while distilled water is added
15 DEG C are warming up to, continues stirring until and is uniformly mixed up to modification of chitosan solution；
Step 4: ferro manganese composite oxides impregnate chitosan beads
By modification of chitosan solution obtained in ferro manganese composite oxides obtained in step 1 and step 3 with mass ratio
The ratio of 2:3 is mixed to high-pressure bottle, by the NaOH solution of 0.2mol/L after high-pressure pump and heat exchanger are heated to 45 DEG C,
It is sprayed into the mixed solution in high-pressure bottle with the speed of 30m/s, adjusting pressure in high-pressure bottle is that 50MPa reacts 3h, is passed through
High-pressure bottle bottom part aperture diameter be 3.5mm filter collect depositing particles, after clean repeatedly with distilled water vacuum drying to get
Ferro manganese composite oxides impregnate chitosan beads adsorbent.
Embodiment 2
A kind of preparation method of ferro manganese composite oxides dipping chitosan beads adsorbent, mainly comprises the steps that
Step 1: ferro manganese composite oxides preparation
Under conditions of magnetic agitation, the KMnO that will arbitrarily buy on the market4Sufficiently melt in deionized water to KMnO4
Concentration is 0.3mol/L, by KMnO4Solution is down in reaction kettle, and control reactor temperature is 25 DEG C, in magnetic agitation condition
Under, dropwise addition and KMnO into reaction kettle430% concentration FeSO of the quality such as solution4Solution after being added dropwise, closes reaction kettle,
Heated solution reacts 1.5h to 115 DEG C under nitrogen atmosphere, and it is 7 that pH value of solution is adjusted after standing to room temperature, centrifugation removal supernatant
Liquid is dried in vacuo 19h at 60-70 DEG C using after dehydrated alcohol and the washing of deionized water alternate repetition, by the precipitating after drying
It is placed in Muffle furnace, the control of Muffle furnace heating rate makes temperature reach 600 DEG C in 2 DEG C/min, roasts 3-4h, grinds after cooling
To 70 mesh, ferro manganese composite oxides are obtained；
Step 2: modifying agent preparation
Take the oxalic acid solution of 1mol/L to mix with the acetic acid solution of 1mol/L with the mass ratio of 1:3, at room temperature with
The hunting of frequency 15min of 10kHz, rapid freezing to 4 DEG C, centrifuging and taking supernatant are added dropwise and supernatant mass ratio into supernatant
For the 0.3mol/L lactic acid solution of 5:1, water-bath 15min in boiling water, it is cooling after up to modifier solution；
Step 3: chitin modified
Modifier solution obtained in chitosan and step 2 is uniformly mixed with the ratio of 2:1 and obtains mixed solution, it will
Mixed solution pressurizes in closed container to be sprayed through 0.5mm spray head, and strong electrical field is arranged around spray head, in forceful electric power field action knit stitch
The mixed solution that head ejects will form taper filamentous, and modified solution is collected through condenser, while distilled water is added
17 DEG C are warming up to, continues stirring until and is uniformly mixed up to modification of chitosan solution；
Step 4: ferro manganese composite oxides impregnate chitosan beads
By modification of chitosan solution obtained in ferro manganese composite oxides obtained in step 1 and step 3 with mass ratio
The ratio of 2:3 is mixed to high-pressure bottle, by the NaOH solution of 0.2mol/L after high-pressure pump and heat exchanger are heated to 47 DEG C,
It is sprayed into the mixed solution in high-pressure bottle with the speed of 35m/s, adjusting pressure in high-pressure bottle is that 50MPa reacts 3h, is passed through
High-pressure bottle bottom part aperture diameter be 3.8mm filter collect depositing particles, after clean repeatedly with distilled water vacuum drying to get
Ferro manganese composite oxides impregnate chitosan beads adsorbent.
Embodiment 3
A kind of preparation method of ferro manganese composite oxides dipping chitosan beads adsorbent, mainly comprises the steps that
Step 1: ferro manganese composite oxides preparation
Under conditions of magnetic agitation, the KMnO that will arbitrarily buy on the market4Sufficiently melt in deionized water to KMnO4
Concentration is 0.3mol/L, by KMnO4Solution is down in reaction kettle, and control reactor temperature is 30 DEG C, in magnetic agitation condition
Under, dropwise addition and KMnO into reaction kettle430% concentration FeSO of the quality such as solution4Solution after being added dropwise, closes reaction kettle,
Heated solution reacts 2h to 120 DEG C under nitrogen atmosphere, and it is 7.5 that pH value of solution is adjusted after standing to room temperature, centrifugation removal supernatant
Liquid is dried in vacuo 20h at 70 DEG C using after dehydrated alcohol and the washing of deionized water alternate repetition, the precipitating after drying is set
In Muffle furnace, the control of Muffle furnace heating rate makes temperature reach 600 DEG C in 2 DEG C/min, roasts 4h, is ground to 80 after cooling
Mesh obtains ferro manganese composite oxides；
Step 2: modifying agent preparation
Take the oxalic acid solution of 1mol/L to mix with the acetic acid solution of 1mol/L with the mass ratio of 1:3, at room temperature with
The hunting of frequency 15min of 10kHz, rapid freezing to 5 DEG C, centrifuging and taking supernatant are added dropwise and supernatant mass ratio into supernatant
For the 0.3mol/L lactic acid solution of 5:1, water-bath 15min in boiling water, it is cooling after up to modifier solution；
Step 3: chitin modified
Modifier solution obtained in chitosan and step 2 is uniformly mixed with the ratio of 2:1 and obtains mixed solution, it will
Mixed solution pressurizes in closed container to be sprayed through 0.5mm spray head, and strong electrical field is arranged around spray head, in forceful electric power field action knit stitch
The mixed solution that head ejects will form taper filamentous, and modified solution is collected through condenser, while distilled water is added
20 DEG C are warming up to, continues stirring until and is uniformly mixed up to modification of chitosan solution；
Step 4: ferro manganese composite oxides impregnate chitosan beads
By modification of chitosan solution obtained in ferro manganese composite oxides obtained in step 1 and step 3 with mass ratio
The ratio of 2:3 is mixed to high-pressure bottle, by the NaOH solution of 0.2mol/L after high-pressure pump and heat exchanger are heated to 50 DEG C,
It is sprayed into the mixed solution in high-pressure bottle with the speed of 40m/s, adjusting pressure in high-pressure bottle is that 50MPa reacts 3h, is passed through
High-pressure bottle bottom part aperture diameter be 4.0mm filter collect depositing particles, after clean repeatedly with distilled water vacuum drying to get
Ferro manganese composite oxides impregnate chitosan beads adsorbent.
Embodiment 4
Difference from example 1 is that: the ferro manganese composite oxides dipping chitosan beads arrived in step 4 are inhaled
Attached dose magnetizes, and obtains magnetic ferro manganese composite oxides dipping chitosan beads adsorbent.
Finally, it should be noted that the above embodiments are merely illustrative of the technical solutions of the present invention, rather than its limitations；To the greatest extent
Present invention has been described in detail with reference to the aforementioned embodiments for pipe, those skilled in the art should understand that: it is still
It can modify to technical solution documented by previous embodiment or equivalent replacement of some of the technical features；
And these are modified or replaceed, technical solution of the embodiment of the present invention that it does not separate the essence of the corresponding technical solution spirit and
Range.
Claims (7)
1. a kind of preparation method of ferro manganese composite oxides dipping chitosan beads adsorbent, which is characterized in that mainly include following
Step:
Step 1: ferro manganese composite oxides preparation
Under conditions of magnetic agitation, by KMnO4Sufficiently melt in deionized water to KMnO4Concentration is 0.3mol/L, will
KMnO4For solution down in reaction kettle, control reactor temperature is 20-30 DEG C, under the conditions of magnetic agitation, is dripped into reaction kettle
Add and KMnO430% concentration FeSO of the quality such as solution4Solution after being added dropwise, is closed reaction kettle, is heated under nitrogen atmosphere
Solution reacts 1-2h to 110-120 DEG C, and it is 6.5-7.5 that pH value of solution is adjusted after standing to room temperature, is centrifuged removal supernatant, repeatedly
It is dried in vacuo 18-20h at 60-70 DEG C after washing, the precipitating after drying is placed in Muffle furnace, control muffle furnace reaches
600 DEG C, 3-4h is roasted, 60-80 mesh is ground to after cooling, obtains ferro manganese composite oxides；
Step 2: modifying agent preparation
The oxalic acid solution of 1mol/L is taken to mix with the acetic acid solution of 1mol/L with the mass ratio of 1:3, at room temperature with the frequency of 10kHz
Rate vibrates 15min, and rapid freezing is to 3-5 DEG C, and centrifuging and taking supernatant, being added dropwise into supernatant with supernatant mass ratio is 5:1's
0.3mol/L lactic acid solution, water-bath 15min in boiling water, it is cooling after up to modifier solution；
Step 3: chitin modified
Modifier solution obtained in chitosan and step 2 is uniformly mixed with the ratio of 2:1 and obtains mixed solution, will be mixed
Solution is sprayed in strong electrical field using electrostatic spinning technique carries out blending and modifying, and modified solution is collected through condenser, is added
It is warming up to 15-20 DEG C while distilled water, continues stirring until and is uniformly mixed up to modification of chitosan solution；
Step 4: ferro manganese composite oxides impregnate chitosan beads
By modification of chitosan solution obtained in ferro manganese composite oxides obtained in step 1 and step 3 with mass ratio 2:3's
Ratio is mixed to high-pressure bottle, by the NaOH solution of 0.2mol/L after high-pressure pump and heat exchanger are heated to 45-50 DEG C, with
The speed of 30-40m/s sprays into the mixed solution in high-pressure bottle, and adjusting pressure in high-pressure bottle is that 50MPa reacts 3h, passes through
The filter of high-pressure bottle bottom collects depositing particles, and vacuum drying is after being cleaned repeatedly with distilled water to get ferrimanganic combined oxidation
Object impregnates chitosan beads adsorbent.
2. a kind of preparation method of ferro manganese composite oxides dipping chitosan beads adsorbent according to claim 1, special
Sign is, the KMnO4For any one the common potassium permanganate that can be bought on the market.
3. a kind of preparation method of ferro manganese composite oxides dipping chitosan beads adsorbent according to claim 1, special
Sign is that the washing repeatedly in the step 1 is alternately washed using dehydrated alcohol and deionized water.
4. a kind of preparation method of ferro manganese composite oxides dipping chitosan beads adsorbent according to claim 1, special
Sign is that the heating rate control of Muffle furnace is 2 DEG C/min in the step 1.
5. a kind of preparation method of ferro manganese composite oxides dipping chitosan beads adsorbent according to claim 1, special
Sign is, the specific steps of electrostatic spinning blending and modifying are carried out in the step 3 are as follows: adds mixed solution in closed container
Pressure is sprayed through 0.5mm spray head, and strong electrical field is arranged around spray head, will form in the mixed solution that forceful electric power field action knit stitch head ejects
Taper filamentous, filamentous is collected through condenser plus distilled water heating fusing.
6. a kind of preparation method of ferro manganese composite oxides dipping chitosan beads adsorbent according to claim 1, special
Sign is that the filter pore size of the high-pressure bottle bottom is 3.5-4.0mm.
7. a kind of preparation method of ferro manganese composite oxides dipping chitosan beads adsorbent according to claim 1, special
Sign is that the washing repeatedly in the step 1 is alternately washed using dehydrated alcohol and deionized water.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114272905A (en) * | 2021-12-14 | 2022-04-05 | 南昌航空大学 | Chitosan-biological iron-manganese oxide material and preparation method and application thereof |
| CN115261151A (en) * | 2022-08-01 | 2022-11-01 | 江西省安智光电科技有限公司 | Cleaning protective agent and application thereof in preparation of touch screen |
| WO2023088982A1 (en) * | 2021-11-18 | 2023-05-25 | Cambridge Enterprise Limited | A process of making an adsorbent body |
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