CN109821510A - A kind of preparation method of chitosan composite adsorbing material - Google Patents
A kind of preparation method of chitosan composite adsorbing material Download PDFInfo
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- CN109821510A CN109821510A CN201910153602.3A CN201910153602A CN109821510A CN 109821510 A CN109821510 A CN 109821510A CN 201910153602 A CN201910153602 A CN 201910153602A CN 109821510 A CN109821510 A CN 109821510A
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Abstract
The present invention relates to a kind of preparation methods of chitosan composite adsorbing material, by AlCl3And MgCl2Mixing is made into primary solution, and NaOH is added, and carries out precipitation reaction, and then ageing is filtered, cleaned, being dried to obtain magnesia aluminum shot；It dissolves the chitosan in acetic acid solution, then the magnesia aluminum shot, ball clay are mixed with the acetic acid solution of chitosan again, and it stirs, atoleine and emulsifier is added, then heat preservation continues stirring a period of time, add the glutaraldehyde that volume fraction is 25%, then it reheats and is reacted, NaOH is added dropwise dropwise simultaneously, the pH value of solution is controlled 9~10, by mixture solution in 70 DEG C of stirred in water bath 1h, solid product is then obtained by high speed centrifugation, solid product is repeatedly washed with deionized water, obtains chitosan composite adsorbing material after dry.Adsorbent material specific surface area of the present invention is larger, porous structure, Selective adsorption are strong, and for adsorbing heavy metal ion, adsorption effect more preferably, belongs to green, safe and environment-friendly material.
Description
Technical field
The present invention relates to environment protection field, specially a kind of preparation method of chitosan composite adsorbing material.
Background technique
Heavy metal refers to density > 4.5g/cm3Metal.Heavy metal pollution is by metallurgy, plating, the discharge of the industries such as process hides
Wastewater in waters and agricultural land soil environment caused by pollute.The danger of heavy metal in water environment to human health and ecological environment
Evil greatly, such as heavy metal Hg, into body after will directly sink to liver, directly destruction brain eyesight is neural；The poison of heavy metal lead
Property is larger, damages to the neural plate of fetus, leads to the diseases such as senile dementia, brain death；Heavy metal chromium will cause human body four
Acroanesthesia, insanity；Metalloid arsenic, it will lead to Skin pigmentation, abnormal keratinization；Cadmium will lead to hypertension and heart and brain
Vascular diseases destroy bone calcium, cause renal dysfunction.The height that heavy metal pollution problem has caused National Environmental Protection Agency is closed
Note makes every effort to control 5 heavy metal species: the discharge amount of mercury, chromium, cadmium, lead and metalloid arsenic in government planning.
Absorption method is concerned in the method for processing heavy metal pollution at present, the adsorbent material that absorption method uses, wherein shell
Glycan contains a large amount of-NH because of its surface2With-COOH isoreactivity group, can be handed over metal ion by chelating and ion
It changes and reacts.Therefore, chitosan becomes research emphasis instantly.
Summary of the invention
The shortcomings that for the above-mentioned prior art, the present invention provide a kind of preparation method of chitosan composite adsorbing material.
The present invention solves above-mentioned technical problem and uses a kind of following technical scheme: preparation side of chitosan composite adsorbing material
Method, comprising the following steps:
(1) by AlCl3And MgCl2It is made into Al3+And Mg2+Molar ratio is the primary solution of 5:4；
(2) NaOH is added dropwise in Xiang Suoshu primary solution, and adjusting solution ph is 11~12, carries out precipitation reaction, makes Al3+
And Mg2+Primary mix is obtained by filtration after being then aged 2h in all precipitatings；
(3) primary mix is cleaned multiple times with deionized water, is then dried to obtain magnesia aluminum shot；
(4) it dissolves the chitosan in acetic acid solution, then again by the second of the magnesia aluminum shot, ball clay and chitosan
Acid solution mixing, and stir, obtain primary mixed solution；
(5) atoleine and emulsifier is added into the primary mixed solution, then heat preservation continues stirring a period of time,
Obtain secondary mixed solution；
(6) glutaraldehyde that volume fraction is 25% is added into the secondary mixed solution, then reheats and carries out instead
It answers, while NaOH being added dropwise dropwise, control the pH value of solution 9~10, obtain whole grade mixed solution；
(7) again by the whole grade mixture solution in 70 DEG C of stirred in water bath 1h, solid is then obtained by high speed centrifugation
Product repeatedly washs solid product with deionized water；
(8) chitosan composite adsorbing material will be obtained after solid product drying.
Preferably, precipitation temperature is 35~45 DEG C in step (2), Aging Temperature is 80~85 DEG C.
Preferably, dry described in step (3) is to be dried in vacuo 12h at 60 DEG C.
Preferably, acetic acid solution volume fraction is 2% in step (4), the matter of chitosan, magnesia aluminum shot and ball clay
Amount is than being (1~2): (2~3): (3~4).
Preferably, stirring described in step (4) is the mechanical stirring that revolving speed is 1500rpm/min, 2~3h is stirred.
Preferably, heat preservation is 30~35 DEG C, insulated and stirred 1h in step (5), the volume ratio of emulsifier and atoleine
For 1:20.
Preferably, being heated to 50 DEG C in step (6), and react 1h.
Preferably, dry described in step (8) is to be dried in vacuo for 24 hours at 70 DEG C.
The invention has the following advantages over the prior art: adsorbent material specific surface area of the present invention is larger, porous structure,
Selective adsorption is strong；Chitosan Composites have the excellent properties such as nontoxic, sterilization, degradable, are excellent heavy metal adsorptions
Material, for adsorbing heavy metal ion, can source to application all meet environmentally protective scope, belong to green, it is safe and environment-friendly
Material；Clay is added in composite adsorbing material of the present invention, enhances the machining property and stability of Chitosan Composites, together
When keep Chitosan Composites enrich functional group, improve its adsorption capacity, adsorption effect is more preferably.
Specific embodiment
In order to be easy to understand the technical means, the creative features, the aims and the efficiencies achieved by the present invention, tie below
Specific embodiment is closed, the present invention is further explained.It should be appreciated that specific embodiment described herein is only used to explain this hair
It is bright, it is not intended to limit the present invention.
Embodiment 1:
By AlCl3And MgCl2It is made into Al3+And Mg2+Molar ratio is the primary solution of 5:4；Add dropwise to the primary solution
Enter NaOH, adjusting solution ph is 11~12, carries out precipitation reaction, and precipitation temperature is 35 DEG C, makes Al3+And Mg2+All precipitatings,
Then primary mix is obtained by filtration after being aged 2h at 80 DEG C；The primary mix is cleaned multiple times with deionized water, then
It is dried in vacuo 12h at 60 DEG C and obtains magnesia aluminum shot.It dissolves the chitosan in the acetic acid solution that volume fraction is 2%, so
The magnesia aluminum shot, ball clay are mixed again with the acetic acid solution of chitosan afterwards, and carry out the machine that revolving speed is 1500rpm/min
Tool stirring, stirs 2h, obtains primary mixed solution；Wherein the mass ratio of chitosan, magnesia aluminum shot and ball clay is 1:2:3.
The volume ratio of addition atoleine and emulsifier into the primary mixed solution, emulsifier and atoleine is 1:20, then
The insulated and stirred 1h at 30 DEG C, obtains secondary mixed solution；Adding volume fraction into the secondary mixed solution is 25%
Glutaraldehyde, be then heated to 50 DEG C, and react 1h, while NaOH being added dropwise dropwise, control the pH value of solution 9~10, obtain
To whole grade mixed solution；Again then the whole grade mixture solution is obtained in 70 DEG C of stirred in water bath 1h by high speed centrifugation
Solid product repeatedly washs solid product with deionized water；The solid product is dried in vacuo at 70 DEG C and obtains shell afterwards for 24 hours
Glycan composite adsorbing material.
Embodiment 2:
By AlCl3And MgCl2It is made into Al3+And Mg2+Molar ratio is the primary solution of 5:4；Add dropwise to the primary solution
Enter NaOH, adjusting solution ph is 11~12, carries out precipitation reaction, and precipitation temperature is 40 DEG C, makes Al3+And Mg2+All precipitatings,
Then primary mix is obtained by filtration after being aged 2h at 83 DEG C；The primary mix is cleaned multiple times with deionized water, then
It is dried in vacuo 12h at 60 DEG C and obtains magnesia aluminum shot.It dissolves the chitosan in the acetic acid solution that volume fraction is 2%, so
The magnesia aluminum shot, ball clay are mixed again with the acetic acid solution of chitosan afterwards, and carry out the machine that revolving speed is 1500rpm/min
Tool stirring, stirs 2.5h, obtains primary mixed solution；Wherein the mass ratio of chitosan, magnesia aluminum shot and ball clay is 1:3:
4.The volume ratio of addition atoleine and emulsifier into the primary mixed solution, emulsifier and atoleine is 1:20, so
The insulated and stirred 1h at 32 DEG C afterwards, obtains secondary mixed solution；Adding volume fraction into the secondary mixed solution is
Then 25% glutaraldehyde is heated to 50 DEG C, and reacts 1h, while NaOH being added dropwise dropwise, control the pH value of solution 9~
10, obtain whole grade mixed solution；Again then the whole grade mixture solution is passed through into high speed centrifugation in 70 DEG C of stirred in water bath 1h
Solid product is obtained, repeatedly washs solid product with deionized water；The solid product is dried in vacuo at 70 DEG C and is obtained afterwards for 24 hours
To chitosan composite adsorbing material.
Embodiment 3:
By AlCl3And MgCl2It is made into Al3+And Mg2+Molar ratio is the primary solution of 5:4；Add dropwise to the primary solution
Enter NaOH, adjusting solution ph is 11~12, carries out precipitation reaction, and precipitation temperature is 45 DEG C, makes Al3+And Mg2+All precipitatings,
Then primary mix is obtained by filtration after being aged 2h at 85 DEG C；The primary mix is cleaned multiple times with deionized water, then
It is dried in vacuo 12h at 60 DEG C and obtains magnesia aluminum shot.It dissolves the chitosan in the acetic acid solution that volume fraction is 2%, so
The magnesia aluminum shot, ball clay are mixed again with the acetic acid solution of chitosan afterwards, and carry out the machine that revolving speed is 1500rpm/min
Tool stirring, stirs 3h, obtains primary mixed solution；Wherein the mass ratio of chitosan, magnesia aluminum shot and ball clay is 2:3:4.
The volume ratio of addition atoleine and emulsifier into the primary mixed solution, emulsifier and atoleine is 1:20, then
The insulated and stirred 1h at 35 DEG C, obtains secondary mixed solution；Adding volume fraction into the secondary mixed solution is 25%
Glutaraldehyde, be then heated to 50 DEG C, and react 1h, while NaOH being added dropwise dropwise, control the pH value of solution 9~10, obtain
To whole grade mixed solution；Again then the whole grade mixture solution is obtained in 70 DEG C of stirred in water bath 1h by high speed centrifugation
Solid product repeatedly washs solid product with deionized water；The solid product is dried in vacuo at 70 DEG C and obtains shell afterwards for 24 hours
Glycan composite adsorbing material.
Embodiment 4:
By AlCl3And MgCl2It is made into Al3+And Mg2+Molar ratio is the primary solution of 5:4；Add dropwise to the primary solution
Enter NaOH, adjusting solution ph is 11~12, carries out precipitation reaction, and precipitation temperature is 42 DEG C, makes Al3+And Mg2+All precipitatings,
Then primary mix is obtained by filtration after being aged 2h at 84 DEG C；The primary mix is cleaned multiple times with deionized water, then
It is dried in vacuo 12h at 60 DEG C and obtains magnesia aluminum shot.It dissolves the chitosan in the acetic acid solution that volume fraction is 2%, so
The magnesia aluminum shot, ball clay are mixed again with the acetic acid solution of chitosan afterwards, and carry out the machine that revolving speed is 1500rpm/min
Tool stirring, stirs 3h, obtains primary mixed solution；Wherein the mass ratio of chitosan, magnesia aluminum shot and ball clay is 1.5:
2.5:3.5.The volume ratio of addition atoleine and emulsifier into the primary mixed solution, emulsifier and atoleine is 1:
20, then the insulated and stirred 1h at 32 DEG C, obtains secondary mixed solution；Volume fraction is added into the secondary mixed solution
For 25% glutaraldehyde, be then heated to 50 DEG C, and react 1h, while NaOH being added dropwise dropwise, control the pH value of solution 9~
10, obtain whole grade mixed solution；Again then the whole grade mixture solution is passed through into high speed centrifugation in 70 DEG C of stirred in water bath 1h
Solid product is obtained, repeatedly washs solid product with deionized water；The solid product is dried in vacuo at 70 DEG C and is obtained afterwards for 24 hours
To chitosan composite adsorbing material.
Basic principles and main features and advantages of the present invention of the invention, the technology of the industry has been shown and described above
Personnel are it should be appreciated that the present invention is not limited to the above embodiments, and the above embodiments and description only describe this
The principle of invention, without departing from the spirit and scope of the present invention, various changes and improvements may be made to the invention, these changes
Change and improvement all fall within the protetion scope of the claimed invention, the claimed scope of the invention by appended claims and its
Equivalent thereof.
Claims (8)
1. a kind of preparation method of chitosan composite adsorbing material, comprising the following steps:
(1) by AlCl3And MgCl2It is made into Al3+And Mg2+Molar ratio is the primary solution of 5:4；
(2) NaOH is added dropwise in Xiang Suoshu primary solution, and adjusting solution ph is 11~12, carries out precipitation reaction, makes Al3+With
Mg2+Primary mix is obtained by filtration after being then aged 2h in all precipitatings；
(3) primary mix is cleaned multiple times with deionized water, is then dried to obtain magnesia aluminum shot；
(4) it dissolves the chitosan in acetic acid solution, it is then again that the acetic acid of the magnesia aluminum shot, ball clay and chitosan is molten
Liquid mixing, and stir, obtain primary mixed solution；
(5) atoleine and emulsifier is added into the primary mixed solution, then heat preservation continues stirring a period of time, obtains
Secondary mixed solution；
(6) glutaraldehyde that volume fraction is 25% is added into the secondary mixed solution, then reheats and reacted, together
When NaOH is added dropwise dropwise, control the pH value of solution 9~10, obtain whole grade mixed solution；
(7) again by the whole grade mixture solution in 70 DEG C of stirred in water bath 1h, solid product is then obtained by high speed centrifugation,
Solid product is repeatedly washed with deionized water；
(8) chitosan composite adsorbing material will be obtained after solid product drying.
2. Aging Temperature is 80~85 DEG C according to the method described in claim 1, precipitation temperature is 35~45 DEG C in step (2).
3. according to the method described in claim 1, dry described in step (3) is to be dried in vacuo 12h at 60 DEG C.
4. chitosan aoxidizes magnalium according to the method described in claim 1, acetic acid solution volume fraction is 2% in step (4)
The mass ratio of grain and ball clay is (1~2): (2~3): (3~4).
5. according to the method described in claim 1, stirring described in step (4) is mechanical stirring that revolving speed is 1500rpm/min,
Stir 2~3h.
6. according to the method described in claim 1, heat preservation is 30~35 DEG C, insulated and stirred 1h in step (5), emulsifier and liquid
The volume ratio of paraffin is 1:20.
7. according to the method described in claim 1, being heated to 50 DEG C in step (6), and reacting 1h.
8. according to the method described in claim 1, dry described in step (8) is to be dried in vacuo for 24 hours at 70 DEG C.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN116688959A (en) * | 2023-06-08 | 2023-09-05 | 南京信息工程大学 | Preparation method and application of nitrogen and phosphorus recovery material |
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Application publication date: 20190531 |