CN106984290A - The preparation method of the chitosan of adsorbing heavy metal ions/sodium alginate magnetic composite microsphere - Google Patents
The preparation method of the chitosan of adsorbing heavy metal ions/sodium alginate magnetic composite microsphere Download PDFInfo
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- CN106984290A CN106984290A CN201710407814.0A CN201710407814A CN106984290A CN 106984290 A CN106984290 A CN 106984290A CN 201710407814 A CN201710407814 A CN 201710407814A CN 106984290 A CN106984290 A CN 106984290A
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- 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
- B01J20/26—Synthetic macromolecular compounds
- B01J20/265—Synthetic macromolecular compounds modified or post-treated polymers
- B01J20/267—Cross-linked polymers
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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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- 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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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/28—Treatment of water, waste water, or sewage by sorption
- C02F1/285—Treatment of water, waste water, or sewage by sorption using synthetic organic sorbents
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
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Abstract
The invention discloses a kind of preparation method of the chitosan of adsorbing heavy metal ions/sodium alginate magnetic composite microsphere, methods described is that will add magnetic nano-particle after chitosan and sodium alginate dissolving to be prepared into mixed solution, then the method bathed using electrostatic drop generation and cooling solidification prepares chitosan/sodium alginate magnetic composite microsphere, and porous chitosan/sodium alginate magnetic composite microsphere is obtained finally by freeze-drying.Magnetic microsphere specific surface area prepared by the present invention is high, and adsorption capacity is big, advantages of good adsorption effect, can adsorb many kinds of metal ions, and convenient recovery.In addition, the raw material sources of complex microsphere are relatively broad, with low cost, preparation technology is simple, with preferable application prospect.
Description
Technical field
The invention belongs to heavy metal ions in wastewater process field, and in particular to a kind of shell of adsorbing heavy metal ions gathers
The preparation method of sugar/sodium alginate magnetic composite microsphere.
Background technology
In recent years, China's economic development is more rapid, but is accompanied by the problem of economic development is brought and is：Machine-building,
The waste water of many heavy metals is all generated in the production process in the fields such as chemical industry, electronic instrument.At present, due to heavy metal processing
Cost is higher, therefore, and heavy metal wastewater thereby is directly discharged into sea or river mostly, and this can cause people to depend on for existence
Water source polluted by heavy metal, such as：Heavy metal ion can be enriched to by food chain in aquatic products product body, so as to make one
Be compromised, in addition, the drinking water of people is conventional treatment mostly, heavy metal ion is probably by drinking water in human body
Interior enrichment.Research shows：Heavy metal ion has larger toxicity：The enzyme system that can be destroyed in human body such as heavy metal, influence
The metabolic activity of human body, causes the generation of the inflammation or edema of human body；In addition, heavy metal ion is also possible to make human body occur weight
Situations such as metal ion is poisoned, has seriously injured the health of the mankind.Therefore, heavy metal ion in sewage disposal is processed into
It is current urgent problem to be solved.
At present, the method for heavy metal removing is mainly the precipitation method, ion-exchange, electrochemical treatment, evaporation in sewage
Freezing method etc., the application of these methods receives the limitation of technique and economic condition.In addition to above-mentioned processing method, absorption
Method is widely used at present, and its technique is relatively simple, and adsorption capacity is big, and can adsorb a variety of different metals from
Son, usually utilizes the microballoon of active group.But, absorption method there is also absorption after microballoon there is also reclaim compared with
The problem of for difficulty.Patent 201410145147.X is carried out using a kind of magnetic bio carbon quantum dot adsorbent heavy metal ion
Absorption, adsorbent prepared by this method has adsorption capacity big, the fast advantage of the rate of adsorption, but there is also preparation cost
High shortcoming；The sodium alginate of patent 201110042318.2, chitosan and and the compound rear and Ca of magnetic nano-particle2+Act on chelant
After be prepared into microsphere adsorbing agent, obtained adsorbent adsorption capacity is stronger, still, and the microballoon that obtains in this way of profit is existed
Sodium alginate and Ca2+Solve the possibility of chelant, the less stable of obtained microballoon.Accordingly, it would be desirable to prepare a kind of adsorption effect compared with
Alright, relatively stable magnetic adsorbent.
The content of the invention
The technical problems to be solved by the invention are to be directed to provide a kind of adsorbable to solve the deficiency of existing process
The preparation method of the chitosan of heavy metal ions in wastewater/sodium alginate magnetic composite microsphere, magnetic microsphere prepared by this method
The problem of adsorbent solves high magnetic microsphere adsorbent cost and poor stability.
In order to solve the above technical problems, the present invention uses following technical scheme：
A kind of preparation method of the chitosan of adsorbing heavy metal ions/sodium alginate magnetic composite microsphere, step is as follows：
（1）Chitosan by deacetylation higher than 80% is dissolved into dilute acid soln, and chitosan adds sea thereto after being completely dissolved
Magnetic nano-particle is added in mosanom, the mixed solution for being sufficiently uniformly dissolved backward chitosan and sodium alginate, magnetic is received
Rice corpuscles is completely dispersed in mixed solution；
（2）By step（1）In added in the mixed solution inhalation syringe of magnetic nano-particle, and on the syringe needle of syringe plus
Upper high-pressure electrostatic, is then squeezed into mixed solution in coagulating bath using syringe pump, obtains chitosan/sodium alginate magnetic coupling micro-
Ball；
（3）By step（2）Obtained chitosan/sodium alginate magnetic composite microsphere is used by filtering from coagulating bath after separation
Glutaraldehyde solution is crosslinked to chitosan/sodium alginate magnetic composite microsphere, complex microsphere is more stablized in aqueous,
After the chitosan after glutaraldehyde cross-linking/sodium alginate magnetic composite microsphere filtering, it is prepared into using freeze-drying porous
The chitosan of adsorbing heavy metal ions/sodium alginate magnetic composite microsphere.
The step（1）The mass ratio of chitosan of the middle deacetylation higher than 80% and sodium alginate is 1:1-1:3.
The step（1）The mass ratio of chitosan of the middle deacetylation higher than 80% and magnetic nano-particle is 1:0.5-1:
1；Described magnetic nano-particle includes but is not limited to rubidium iron boron nano-particle, ferriferrous oxide nano-particle.
The step（1）In dilute acid soln be that the acetum that volumetric concentration is 1% or the hydrochloric acid that volumetric concentration is 1% are molten
Liquid.
The step（2）In coagulating bath be 0.1mol/L-1mol/L NaOH solution.
The step（2）In voltage added on syringe needle be 5kV-20kV；The speed of syringe pump is 200mL/h
-500mL/h。
The step（3）Glutaraldehyde solution volumetric concentration（v/v）For 1%-5%, chitosan/sodium alginate magnetic coupling
Mass-volume concentration of the microballoon in glutaraldehyde solution is 0.2g/mL-1g/mL.
The step（3）The temperature of middle freeze-drying is -40 DEG C, and the time of freeze-drying is 24-48h.
It is multiple made from the preparation method of the chitosan of described adsorbing heavy metal ions/sodium alginate magnetic composite microsphere
Close application of the microballoon in heavy metal ions in wastewater processing.
Compared with prior art, beneficial effects of the present invention are as follows：
After the present invention is combined using chitosan, sodium alginate and magnetic particle, had using electrostatic drop generation, freeze-drying
There is the complex microsphere of loose structure, raw material relatively broad, with low cost advantage high with adsorption efficiency, and it is obtained micro-
Ball adsorbent has specific surface area big, and environmental protection, free of contamination feature can adsorb many kinds of metal ions, and adsorbent
Reclaim relatively simple, with good renewable.
Embodiment
With reference to specific embodiment, the present invention will be further described.It should be understood that following examples are merely to illustrate this
Invention can make one not for limitation the scope of the present invention, the person skilled in the art in the field according to the content of foregoing invention
A little nonessential modifications and adaptations.
Embodiment 1
The preparation method of the chitosan of the adsorbing heavy metal ions of the present embodiment/sodium alginate magnetic composite microsphere, step is such as
Under：
（1）1g deacetylations are dissolved into 200mL dilute hydrochloric acid solutions for 85% chitosan（v/v=1%）In, chitosan is completely molten
1g sodium alginates are added after solution thereto, 0.5g is added in the mixed solution for being sufficiently uniformly dissolved backward chitosan and sodium alginate
Rubidium iron boron magnetic nano-particle, makes magnetic nano-particle be completely dispersed in mixed solution；
（2）By in mixed solution inhalation syringe, and syringe is fixed on syringe pump, on syringe needle plus 5kV
Mixed solution, is then squeezed into 0.1mol/L NaOH coagulating baths and obtains chitosan/sea by electrostatic with 200mL/h speed
Mosanom magnetic composite microsphere；
（3）After obtained magnetic composite microsphere is filtered, 10g is taken to be added to 10mL 1%（v/v）Glutaraldehyde solution in, crosslinking
After fixed 2h, microballoon is filtered, 24h is freeze-dried under conditions of -40 DEG C and obtains adsorbing heavy metal ions（It is porous）Shell
Glycan/sodium alginate magnetic composite microsphere.
Embodiment 2
The preparation method of the chitosan of the adsorbing heavy metal ions of the present embodiment/sodium alginate magnetic composite microsphere, step is such as
Under：
（1）1g deacetylations are dissolved into 100mL dilute acetic acid solutions for 85% chitosan（v/v=1%）In, chitosan is completely molten
2g sodium alginates are added after solution thereto, addition 1g rubidiums in the mixed solution of backward chitosan and sodium alginate are sufficiently uniformly dissolved
Iron boron magnetic nano-particle, makes magnetic nano-particle be completely dispersed in mixed solution；
（2）By in mixed solution inhalation syringe, and syringe is fixed on syringe pump, on syringe needle plus 10kV
Mixed solution, is then squeezed into 0.5mol/L NaOH coagulating baths and obtains chitosan/sea by electrostatic with 300mL/h speed
Mosanom magnetic composite microsphere；
（3）After obtained magnetic composite microsphere is filtered, 2g is taken to be added to 10mL 3%（v/v）Glutaraldehyde solution（Fixer）
In, after the fixed 2h of crosslinking, microballoon is filtered, 48h is freeze-dried under conditions of -40 DEG C and obtains adsorbing heavy metal ions（It is many
Hole）Chitosan/sodium alginate magnetic composite microsphere.
Embodiment 3
The preparation method of the chitosan of the adsorbing heavy metal ions of the present embodiment/sodium alginate magnetic composite microsphere, step is such as
Under：
（1）1g deacetylations are dissolved into 200mL dilute hydrochloric acid solutions for 85% chitosan（v/v=1%）In, chitosan is completely molten
3g sodium alginates are added after solution thereto, addition 1g tetra- in the mixed solution of backward chitosan and sodium alginate is sufficiently uniformly dissolved
Fe 3 O magnetic nano-particle, makes magnetic nano-particle be completely dispersed in mixed solution；
（2）By in mixed solution inhalation syringe, and syringe is fixed on syringe pump, on syringe needle plus 20kV
Mixed solution, is then squeezed into and obtains shell in 1mol/L NaOH coagulating bath solidify liquids and gather by electrostatic with 500mL/h speed
Sugar/sodium alginate magnetic composite microsphere；
（3）After obtained magnetic composite microsphere is filtered, 5g is taken to be added to 10mL 5%（v/v）Glutaraldehyde fixer in, it is fixed
After 2h, microballoon is filtered, 36h is freeze-dried under conditions of -40 DEG C and obtains adsorbing heavy metal ions（It is porous）Chitosan/
Sodium alginate magnetic composite microsphere.
Embodiment 4
The preparation method of the chitosan of the adsorbing heavy metal ions of the present embodiment/sodium alginate magnetic composite microsphere, step is such as
Under：
（1）1g deacetylations are dissolved into 200mL dilute acetic acid solutions for 85% chitosan（v/v=1%）In, chitosan is completely molten
2g sodium alginates are added after solution thereto, 0.5g is added in the mixed solution for being sufficiently uniformly dissolved backward chitosan and sodium alginate
Rubidium iron boron magnetic nano-particle, makes magnetic nano-particle be completely dispersed in mixed solution；
（2）By in mixed solution inhalation syringe, and syringe is fixed on syringe pump, on syringe needle plus 20kV
Mixed solution, is then squeezed into 0.5mol/L NaOH coagulating baths and obtains chitosan/sea by electrostatic with 200mL/h speed
Mosanom magnetic composite microsphere；
（3）After obtained magnetic composite microsphere is filtered, 8g is taken to be added to 10mL 5%（v/v）Glutaraldehyde fixer in, crosslinking
After fixed 2h, microballoon is filtered, 30h is freeze-dried under conditions of -40 DEG C and obtains adsorbing heavy metal ions（It is porous）Shell
Glycan/sodium alginate magnetic composite microsphere.
The general principle and principal character and advantages of the present invention of the present invention has been shown and described above.The skill of the industry
Art personnel are it should be appreciated that the present invention is not limited to the above embodiments, and described in above-described embodiment and specification is explanation
The principle of the present invention, without departing from the spirit and scope of the present invention, various changes and modifications of the present invention are possible, these
Changes and improvements all fall within the protetion scope of the claimed invention.The claimed scope of the invention by appended claims and
Its equivalent thereof.
Claims (9)
1. a kind of preparation method of the chitosan of adsorbing heavy metal ions/sodium alginate magnetic composite microsphere, it is characterised in that
Step is as follows：
（1）Chitosan by deacetylation higher than 80% is dissolved into dilute acid soln, and chitosan adds sea thereto after being completely dissolved
Magnetic nano-particle is added in mosanom, the mixed solution for being sufficiently uniformly dissolved backward chitosan and sodium alginate, magnetic is received
Rice corpuscles is completely dispersed in mixed solution；
（2）By step（1）In added in the mixed solution inhalation syringe of magnetic nano-particle, and on the syringe needle of syringe plus
Upper high-pressure electrostatic, is then squeezed into mixed solution in coagulating bath using syringe pump, obtains chitosan/sodium alginate magnetic coupling micro-
Ball；
（3）By step（2）Obtained chitosan/sodium alginate magnetic composite microsphere is used by filtering from coagulating bath after separation
Glutaraldehyde solution is crosslinked to chitosan/sodium alginate magnetic composite microsphere, complex microsphere is more stablized in aqueous,
After the chitosan after glutaraldehyde cross-linking/sodium alginate magnetic composite microsphere filtering, it is prepared into using freeze-drying porous
The chitosan of adsorbing heavy metal ions/sodium alginate magnetic composite microsphere.
2. the preparation of the chitosan of adsorbing heavy metal ions according to claim 1/sodium alginate magnetic composite microsphere
Method, it is characterised in that：The step（1）The mass ratio of chitosan of the middle deacetylation higher than 80% and sodium alginate is 1:1-
1:3。
3. the preparation of the chitosan of adsorbing heavy metal ions according to claim 1/sodium alginate magnetic composite microsphere
Method, it is characterised in that：The step（1）Middle deacetylation is higher than 80% chitosan and the mass ratio of magnetic nano-particle is
1:0.5-1:1；Described magnetic nano-particle includes but is not limited to rubidium iron boron nano-particle, ferriferrous oxide nano-particle.
4. the preparation of the chitosan of adsorbing heavy metal ions according to claim 1/sodium alginate magnetic composite microsphere
Method, it is characterised in that：The step（1）In dilute acid soln be acetum that volumetric concentration is 1% or volumetric concentration is 1%
Hydrochloric acid solution.
5. the preparation of the chitosan of adsorbing heavy metal ions according to claim 1/sodium alginate magnetic composite microsphere
Method, it is characterised in that：The step（2）In coagulating bath be 0.1mol/L-1mol/L NaOH solution.
6. the preparation of the chitosan of adsorbing heavy metal ions according to claim 1/sodium alginate magnetic composite microsphere
Method, it is characterised in that：The step（2）In voltage added on syringe needle be 5kV-20kV；The speed of syringe pump
For 200mL-500mL/h.
7. the preparation of the chitosan of adsorbing heavy metal ions according to claim 1/sodium alginate magnetic composite microsphere
Method, it is characterised in that：The step（3）Glutaraldehyde solution volumetric concentration be 1%-5%, chitosan/sodium alginate magnetic
Mass-volume concentration of the complex microsphere in glutaraldehyde solution is 0.2g/mL-1g/mL.
8. the preparation of the chitosan of adsorbing heavy metal ions according to claim 1/sodium alginate magnetic composite microsphere
Method, it is characterised in that：The step（3）The temperature of middle freeze-drying is -40 DEG C, and the time of freeze-drying is 24-48h.
9. according to chitosan/sodium alginate magnetic composite microsphere of any described adsorbing heavy metal ions of claim 1 ~ 8
Preparation method made from complex microsphere heavy metal ions in wastewater processing in application.
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| CN107722991A (en) * | 2017-10-31 | 2018-02-23 | 中国环境科学研究院 | A kind of heavy metal-polluted soil pollution of chromium repair materials and preparation method and application |
| CN107936285A (en) * | 2017-11-28 | 2018-04-20 | 福建省致青生态环保有限公司 | The Preparation method and use of magnetic ferroferric oxide polylactic acid composite porous microspheres |
| CN108176370A (en) * | 2017-12-22 | 2018-06-19 | 苏州纳贝通环境科技有限公司 | A kind of preparation method of magnetic gel heavy metal absorbent |
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