CN109225155A - A kind of preparation method of the superior adsorbent for cerium ion recycling - Google Patents
A kind of preparation method of the superior adsorbent for cerium ion recycling Download PDFInfo
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- CN109225155A CN109225155A CN201811259957.2A CN201811259957A CN109225155A CN 109225155 A CN109225155 A CN 109225155A CN 201811259957 A CN201811259957 A CN 201811259957A CN 109225155 A CN109225155 A CN 109225155A
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- adsorbent
- cerium ion
- ion recycling
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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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- 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
- C02F1/286—Treatment of water, waste water, or sewage by sorption using natural organic sorbents or derivatives thereof
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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
-
- 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
- C02F2101/10—Inorganic compounds
- C02F2101/20—Heavy metals or heavy metal compounds
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Abstract
The invention discloses a kind of preparation methods of superior adsorbent for cerium ion recycling, it realizes by the one-step method preparation of krill shell to improvement chitin adsorbent, the improvement chitin adsorbent of preparation has extraordinary absorption property to Ce (IV).Compared with existing utilization prepares the method for shrimp and crab shells preparation improvement chitosan absorbent, it is multiple to have the advantages that preparation process is simple, short, the low in cost and product characters of time-consuming are excellent etc..
Description
Technical field
The present invention relates to shrimp shell processing technique fields, and in particular to a kind of system of the superior adsorbent for cerium ion recycling
Preparation Method.
Background technique
Ce elements are a kind of rare earth elements, belong to national strategy resource, and recycling has been put into country's weight with using technology
Point brainstorm subject.There is extraordinary adsorption effect to cerium ion (Ce (IV)) after chitosan class adsorbent is improved.Chitosan
Class adsorbent is mainly by shrimp shell, crab shell through the processes preparation such as decalcification, de- albumen, deacetylated, complex process, with high costs.
It has been investigated that the shell using krill can be by the chitin adsorbent of single step reaction preparation improvement.As one kind
Completely new technical method has not yet to see correlative study report.
Summary of the invention
Object of the present invention is to: a kind of preparation method of superior adsorbent for cerium ion recycling is provided, it is above-mentioned to solve
Problem.
The technical scheme is that
A kind of preparation method of the superior adsorbent for cerium ion recycling, this method comprises the following steps:
(1) shell of krill is dry, removal of impurities, is crushed with micronizer, obtains shrimp shell meal；
(2) shrimp shell meal is transferred to reactor, disodium EDTA solution, azodiisobutyronitrile solution is added
With cyclohexanone peroxide solution, solution ph is adjusted, sealing continuously stirs under infrared heating, obtains product；
(3) product is filtered, takes filter residue to be washed with water to neutrality, vacuum drying can be obtained the first of EDTA functionalization
Shell element adsorbent.
Further, crushing described in step (1) needs so that shrimp shell meal crosses 200 mesh screens.
Further, the final concentration of 5-15%, m/v of disodium EDTA solution described in step (2).
Further, the final concentration of 0.1-10%, m/v of azodiisobutyronitrile solution described in step (2).
Further, the final concentration of 1-5%, m/v of cyclohexanone peroxide solution described in step (2).
Further, pH value range described in step (2) is 10-12.
Further, the temperature of infrared heating described in step (2) is 40-60 DEG C.
Further, the revolving speed continuously stirred described in step (2) is 160-180rpm, and temperature is 60-80 DEG C, and the time is
1-10h。
Further, filtering described in step (3) is filtered under vacuum pump auxiliary using neutral filter paper.
Further, vacuum drying temperature described in step (3) is 65 DEG C, time 40-50h.
The present invention provides a kind of preparation methods of superior adsorbent for cerium ion recycling, realize by krill
To the one-step method preparation of improvement chitin adsorbent, the improvement chitin adsorbent of preparation has Ce (IV) extraordinary shell
Absorption property.Compared with existing utilization prepares the method for shrimp and crab shells preparation improvement chitosan absorbent, simple with preparation process,
Multiple advantages such as time-consuming short, low in cost and product characters are excellent.
Detailed description of the invention
Fig. 1 is the electron microscope scanning figure of commercial chitin；
Fig. 2 is crust prepared by a kind of preparation method of superior adsorbent for cerium ion recycling provided by the invention
The electron microscope scanning figure of element；
Fig. 3 is crust prepared by a kind of preparation method of superior adsorbent for cerium ion recycling provided by the invention
Plain adsorbent13C-NMR figure；
Fig. 4 is that commodity chitin adsorbs Ce4+Element mapping graph afterwards；
Fig. 5 is crust prepared by a kind of preparation method of superior adsorbent for cerium ion recycling provided by the invention
Element absorption Ce4+Element mapping graph afterwards.
Specific embodiment
In order to make the foregoing objectives, features and advantages of the present invention clearer and more comprehensible, With reference to embodiment
And the present invention is described in further detail for attached drawing.
A kind of preparation method of the superior adsorbent for cerium ion recycling, comprising:
Step 1: the shell of krill is dry, removal of impurities is crushed with micronizer, obtains shrimp shell meal；
The step specific as follows can execute: the shell of krill is dry, removal of impurities is crushed, mistake with micronizer
200 mesh screens obtain shrimp shell meal.
Step 2: the shrimp shell meal is transferred to reactor, disodium EDTA solution, azodiisobutyronitrile is added
Solution and cyclohexanone peroxide solution adjust solution ph, and sealing continuously stirs under infrared heating, obtain product；
The step specific as follows can execute: the shrimp shell meal being transferred to reactor, final concentration of 5-15% (m/v) is added
Disodium EDTA solution, final concentration of 0.1-10% (m/v) azodiisobutyronitrile solution and final concentration of 1-5%
(m/v) cyclohexanone peroxide solution adjusts solution ph 10-12, and sealing, 40-60 DEG C of infrared heating, be 160- in revolving speed
180rpm, temperature continuously stir 1-10h under conditions of being 60-80 DEG C, obtain product.
Step 3: the product is filtered, and takes filter residue to be washed with water to neutrality, vacuum drying can be obtained EDTA functionalization
Chitin adsorbent；
The step specific as follows can execute: by the product using neutral filter paper, filtering under vacuum pump auxiliary, take filter
Slag is washed with water to neutrality, is dried in vacuo 40-50h under conditions of temperature is 65 DEG C, can be obtained the chitin of EDTA functionalization
Adsorbent.
There is micro-nano hole gap structure by chitin adsorbent obtained by the above method, carbon composes solid-state nuclear magnetic resonance
(13C-NMR) technology confirms that its main component is chitin, and by EDTA functionalization.Remaining performance please refers to Fig. 1 to Fig. 5:
Fig. 1 is commodity chitin adsorbent, and Fig. 2 is the chitin adsorbent of this method preparation, can from Fig. 1 and Fig. 2
Out, commodity chitin adsorbent does not have apparent pore structure, and the functionalization chitin adsorbent of this method preparation is with bright
Aobvious micro-nano hole gap structure.
Fig. 3 is that the carbon of the chitin adsorbent (EP) of commodity chitin adsorbent (CP) and this method preparation composes solid state nmr
Resonate (13C-NMR) map, as seen from Figure 3 the chitin adsorbent (EP) of this method preparation 22.62,73.27,
75.34, the characteristic peak on chitin is shown at 82.80 and 103.93, shows that its main structure is chitin；55.01,
The characteristic peak of EDTA is shown at 60.35 and 174.25, the appearance at these peaks has proved the chitin adsorbent of this method preparation
Through success by EDTA functionalization, belong to a kind of novel substance.
Fig. 4 is the element mapping graph of commodity chitin adsorbent (CP), and Fig. 5 is the chitin adsorbent of this method preparation
(EP) the element mapping graph of Ce elements on is said it can readily be seen that the cerium of CP absorption is significantly lower than EP from Fig. 4 and Fig. 5
Bright EP is significantly higher than CP to the adsorption capacity of cerium.
In order to make the foregoing objectives, features and advantages of the present invention clearer and more comprehensible, further below with reference to embodiment
Illustrate technical solution of the present invention.But the present invention is not limited to listed embodiments, should also be included in of the presently claimed invention
Other any well known changes in interest field.
" one embodiment " or " embodiment " referred to herein, which refers to, may be included at least one implementation of the invention
A particular feature, structure, or characteristic." in one embodiment " that different places occur in the present specification not refers both to same
A embodiment, nor the individual or selective embodiment mutually exclusive with other embodiments.
Embodiment 1
The implementation case shows a kind of preparation method of superior adsorbent for cerium ion recycling as follows: will be southern
The shell of pole krill is dry, cleans, and is crushed with micronizer, crosses 200 mesh screens, obtains shrimp shell meal.Shrimp shell meal is transferred to instead
Device is answered, disodium EDTA solution (EDTA, 5%, m/v), azodiisobutyronitrile solution (0.1%), peroxidating is added
Cyclohexanone solution (1%) adjusts solution ph to 10-12, seals, is 160rpm, temperature in revolving speed under infrared heating (40 DEG C)
1h is continuously stirred under conditions of being 60 DEG C, product is filtered, filter residue is washed with water into using neutral filter paper under vacuum pump auxiliary
Property, it is dried in vacuo 40h under conditions of temperature is 65 DEG C, can be obtained final product, the chitin adsorbent of EDTA functionalization.
Experiment shows that it reaches as high as 151.02mg/g to the adsorption capacity of cerium ion (Ce-IV).
Embodiment 2
The implementation case shows a kind of preparation method of superior adsorbent for cerium ion recycling as follows:
The shell of krill is dry, removal of impurities, is crushed with micronizer, crosses 200 mesh screens, obtains shrimp shell meal.It will
Shrimp shell meal is transferred to reactor, and disodium EDTA solution (EDTA, 10%, m/v), azodiisobutyronitrile solution is added
(5%, m/v), cyclohexanone peroxide solution (3%, m/v) adjust solution ph to 11, and sealing, infrared heating (50 DEG C) is turning
Speed is 170rpm, temperature continuously stirs 6h under conditions of being 70 DEG C, and product is filtered under vacuum pump auxiliary using neutral filter paper,
Filter residue is washed with water to neutrality, is dried in vacuo 45h under conditions of temperature is 65 DEG C, can be obtained final product, EDTA functionalization
Chitin adsorbent.
Experiment shows that it reaches as high as 154.74mg/g to the adsorption capacity of cerium ion (Ce-IV).
Embodiment 3
The implementation case shows a kind of preparation method of superior adsorbent for cerium ion recycling as follows:
The shell of krill is dry, removal of impurities, is crushed with micronizer, crosses 200 mesh screens, obtains shrimp shell meal.It will
Shrimp shell meal is transferred to reactor, and disodium EDTA solution (EDTA, 15%, m/v), azodiisobutyronitrile solution is added
(10%, m/v), cyclohexanone peroxide solution (5%, m/v), adjusting solution ph to 12, sealing, infrared heating (60 DEG C),
Revolving speed is 180rpm, temperature continuously stirs 10h under conditions of being 80 DEG C, and product is using neutral filter paper, the mistake under vacuum pump auxiliary
Filter, filter residue are washed with water to neutrality, are dried in vacuo 50h under conditions of temperature is 65 DEG C, can be obtained final product, EDTA function
The chitin adsorbent of change.
Experiment shows that it reaches as high as 139.08mg/g to the adsorption capacity of cerium ion (Ce-IV).
Comparative example 1
The implementation case shows a kind of preparation method of superior adsorbent for cerium ion recycling as follows:
The shell of swimming crab is dry, removal of impurities, is crushed with micronizer, crosses 200 mesh screens, obtains shrimp shell meal.By shrimp
Shell powder is transferred to reactor, and disodium EDTA (EDTA, 10%, m/v), azodiisobutyronitrile (5%), peroxidating is added
Cyclohexanone (3%) adjusts solution ph to 11, seals, 6h, product filtering are continuously stirred under infrared heating (50 DEG C), filter residue is used
It is washed to neutrality, is dried in vacuo, can be obtained final product, the chitin adsorbent of EDTA functionalization.
Experiment shows that it reaches as high as 154.74mg/g to the adsorption capacity of cerium ion (Ce-IV).
Following table 1 is the comparison of 4 embodiments and present technology, specific as follows:
Table 1
Compared with prior art, the beneficial effects of the present invention are: simple process, highly-safe, production cost is low, adsorptivity
It can be good.
It should be noted that the above examples are only used to illustrate the technical scheme of the present invention and are not limiting, although referring to preferable
Embodiment describes the invention in detail, those skilled in the art should understand that, it can be to technology of the invention
Scheme is modified or replaced equivalently, and without departing from the spirit and scope of the technical solution of the present invention, should all be covered in this hair
In bright scope of the claims.
Claims (10)
1. a kind of preparation method of the superior adsorbent for cerium ion recycling, which is characterized in that this method comprises the following steps:
(1) shell of krill is dry, removal of impurities, is crushed with micronizer, obtains shrimp shell meal；
(2) shrimp shell meal is transferred to reactor, disodium EDTA solution, azodiisobutyronitrile solution and mistake is added
Peroxyester solution adjusts solution ph, and sealing continuously stirs under infrared heating, obtains product；
(3) product is filtered, takes filter residue to be washed with water to neutrality, vacuum drying can be obtained the chitin of EDTA functionalization
Adsorbent.
2. a kind of preparation method of superior adsorbent for cerium ion recycling according to claim 1, it is characterised in that:
Crushing described in step (1) needs so that shrimp shell meal crosses 200 mesh screens.
3. a kind of preparation method of superior adsorbent for cerium ion recycling according to claim 1, it is characterised in that:
The final concentration of 5-15%, m/v of disodium EDTA solution described in step (2).
4. a kind of preparation method of superior adsorbent for cerium ion recycling according to claim 1, it is characterised in that:
The final concentration of 0.1-10%, m/v of azodiisobutyronitrile solution described in step (2).
5. a kind of preparation method of superior adsorbent for cerium ion recycling according to claim 1, it is characterised in that:
The final concentration of 1-5%, m/v of cyclohexanone peroxide solution described in step (2).
6. a kind of preparation method of superior adsorbent for cerium ion recycling according to claim 1, it is characterised in that:
PH value range described in step (2) is 10-12.
7. a kind of preparation method of superior adsorbent for cerium ion recycling according to claim 1, it is characterised in that:
The temperature of infrared heating described in step (2) is 40-60 DEG C.
8. a kind of preparation method of superior adsorbent for cerium ion recycling according to claim 1, it is characterised in that:
The revolving speed continuously stirred described in step (2) is 160-180rpm, and temperature is 60-80 DEG C, time 1-10h.
9. a kind of preparation method of superior adsorbent for cerium ion recycling according to claim 1, it is characterised in that:
Filtering described in step (3) is filtered under vacuum pump auxiliary using neutral filter paper.
10. a kind of preparation method of superior adsorbent for cerium ion recycling according to claim 1, feature exist
In vacuum drying temperature described in step (3) is 65 DEG C, time 40-50h.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN110343274A (en) * | 2019-07-18 | 2019-10-18 | 浙江海洋大学 | A kind of preparation method of bright enhancement film transparent substrates |
| CN111250065A (en) * | 2019-10-10 | 2020-06-09 | 浙江海洋大学 | Preparation method and application of EDTA (ethylene diamine tetraacetic acid) modified mussel shell powder |
| CN113121720A (en) * | 2019-12-30 | 2021-07-16 | 中国科学院理化技术研究所 | Modified chitin and application thereof in enrichment of artificial radionuclide |
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| CN111250065A (en) * | 2019-10-10 | 2020-06-09 | 浙江海洋大学 | Preparation method and application of EDTA (ethylene diamine tetraacetic acid) modified mussel shell powder |
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Application publication date: 20190118 |