CN106311163B - A kind of preparation method of the chitosan of arsenic-adsorbing/iron hydroxide compound adsorbent - Google Patents
A kind of preparation method of the chitosan of arsenic-adsorbing/iron hydroxide compound adsorbent Download PDFInfo
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- CN106311163B CN106311163B CN201610850199.6A CN201610850199A CN106311163B CN 106311163 B CN106311163 B CN 106311163B CN 201610850199 A CN201610850199 A CN 201610850199A CN 106311163 B CN106311163 B CN 106311163B
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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
- B01J20/02—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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- 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
- C02F1/281—Treatment of water, waste water, or sewage by sorption using inorganic 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
- 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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- 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
- C02F2101/103—Arsenic compounds
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- Environmental & Geological Engineering (AREA)
- Water Supply & Treatment (AREA)
- Inorganic Chemistry (AREA)
- Analytical Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Polysaccharides And Polysaccharide Derivatives (AREA)
- Solid-Sorbent Or Filter-Aiding Compositions (AREA)
Abstract
The present invention is directed to existing environmental problem, provides chitosan/iron hydroxide compound adsorbent and preparation method thereof that a kind of pair of arsenic has high adsorption effect.It first uses ferric chloride in aqueous solution to dissolve chitosan for solvent, then sodium hydroxide solution is added dropwise in dissolution acquired solution, in-situ preparation chitosan/ferric hydroxide composite adds glutaraldehyde solution crosslinking, chitosan/iron hydroxide adsorbent can be obtained.Preparation method of the present invention is economic and environment-friendly, and can realize compound on chitosan and iron hydroxide molecular level, is conducive to be prepared the adsorbent for having high adsorption effect to arsenic.
Description
Technical field
The present invention relates to a kind of chitosan of arsenic-adsorbing/iron hydroxide compound adsorbent preparation methods, belong to chemical industry skill
Art field.
Background technique
Heavy metal ion pollution problem in water body is always important environmental problem urgently to be resolved.In the heavy metal of water
In pollution, arsenic ion is more prominent with its strong toxicity.Arsenic is commonly referred to as the king of poisonous substance.Arsenic from underwater content is exceeded
It is the important problem for perplexing countries in the world.The World Health Organization it is recommended that Arsenic in Drinking Water content no more than 0.01 mg/L.
Arsenic is all exceeded in the ground such as China Inner Mongol, Shanxi, Xinjiang underground drinking water at present.Therefore the water process exceeded to arsenic content reduces
Its arsenic concentration has great importance.
A variety of methods that arsenic is removed from water are developed at present, comprising: oxidation-precipitation method, condensation-flocculence, film exchange
Method, absorption method and nanof iotaltration etc..Absorption method technique is most simple in these methods, and cost consumption is minimum, therefore and most by
It is widely applied, is the important method handled currently used for arsenic in water.When carrying out adsorption treatment to arsenic in water using absorption method, inhale
Attached dose of preparation and performance are mostly important.A large amount of new adsorbent occurs successively, as activated aluminum, active carbon, hydroxyapatite,
Rare-earth oxide, molecular sieve etc..But existing adsorbent is not able to satisfy requirement still, high, preparation that there are manufacturing costs
The disadvantages such as complex process, adsorbance be low.Chitosan is from a wealth of sources, and cost is relatively low, and contains amino in chitosan molecule chain, so that
Chitosan has preferable adsorption effect to metal ion etc..But chitosan is limited to the adsorption efficiency of arsenic (V), it is difficult to as
The high-efficiency adsorbent of arsenic uses, and need to be modified to chitosan.Common method of modifying is that have chitosan and others to arsenic
There is the component of high adsorption effect compound.Early-stage study shows that Arsenic By Ferric Hydroxide has preferable adsorption effect, as can by hydroxide
Iron is supported on chitosan, is expected to that the compound adsorbent for having high adsorption effect to arsenic is prepared.
To prepare chitosan/iron hydroxide compound adsorbent that a kind of pair of arsenic has high adsorption, invention one
Kind chitosan/iron hydroxide compound adsorbent preparation method.
Summary of the invention
The present invention is directed to existing environmental problem, provides chitosan/iron hydroxide that a kind of pair of arsenic has high adsorption effect
Compound adsorbent and preparation method thereof.Ferric chloride in aqueous solution is first used to dissolve chitosan for solvent, then in dissolution acquired solution
Sodium hydroxide solution is added dropwise, in-situ preparation chitosan/ferric hydroxide composite adds glutaraldehyde solution crosslinking, can be obtained
Chitosan/iron hydroxide adsorbent.
The purpose of the present invention is what is realized by following technical measures, wherein the raw material score is unless otherwise specified, it is
Weight fraction.
A kind of preparation method of chitosan/iron hydroxide compound adsorbent:
(1) selecting ferric chloride in aqueous solution is the solvent of chitosan, iron chloride is made into the aqueous solution of 2 ~ 5 wt%, in 60-90
Chitosan is dissolved by heating in DEG C water-bath obtains the chitosan solution of 2-5 wt%.
(2) chitosan/ferric chloride solution in (1) is gradually added dropwise to 5 ~ 10 wt% sodium hydroxide solutions again, it is poly- to generate shell
Sugar/bulky ferric hydroxide precipitate.The volume mass of sodium hydroxide solution and chitosan ratio is 10 ~ 20 mL:1 g.
(3) by chitosan/bulky ferric hydroxide precipitate obtained in (2) be added to 5 ~ 10 wt% glutaraldehyde or epichlorohydrin it is molten
In liquid at 30 ~ 60 DEG C 2 h of cross-linking reaction, by gained be crosslinked chitosan/iron hydroxide rinsed with deionized water, with remove
Chitosan/iron hydroxide adsorbent can be obtained in unreacted glutaraldehyde or epichlorohydrin；Glutaraldehyde or epichlorohydrin solution and shell are poly-
The volume mass ratio of sugar is 10 ~ 20 mL:1 g；
(4) above-mentioned gained chitosan/iron hydroxide solid is dry in freeze drier, after obtaining solid cementitious material
Partial size is ground to less than 1000 μm to get the chitosan/iron hydroxide compound adsorbent to arsenic with high adsorption.
Directly selecting ferric chloride in aqueous solution is the solvent of chitosan, avoids the use of chitosan conventional solvent acetic acid.?
After dissolving chitosan in ferric chloride in aqueous solution, sodium hydroxide solution is added, so that the iron chloride in solution is converted into hydrogen-oxygen
Change iron, generates chitosan/iron hydroxide composite precipitation.
The present invention directlys adopt ferric chloride in aqueous solution dissolution chitosan, and generates ferric hydroxide precipitate in situ, obtains shell
Glycan/ferric hydroxide composite, present invention process route is simple, and the composite adsorption for having high adsorption effect to arsenic can be prepared
Agent.
The present invention has the advantage that
(1) the use of ferric chloride in aqueous solution is chitosan solvent, the use of the conventional solvent acetic acid of chitosan is avoided, molten
It can preferably protect chitosan non-degradable in solution preocess.
(2) upon dissolution, sodium hydroxide solution is added dropwise in the solution, so that the iron chloride in solution is converted into iron hydroxide
Precipitating, and chitosan is precipitated, obtain chitosan/ferric hydroxide precipitate.
(3) in the present invention, iron chloride both provides solute effect to chitosan, also can be used as the presoma of iron hydroxide
It uses.The preparation method of adsorbent is economic and environment-friendly, and can realize compound on chitosan and iron hydroxide molecular level, is conducive to
The adsorbent for having high adsorption effect to arsenic is prepared.
Specific embodiment
The present invention is specifically described below by specific embodiment.It is necessarily pointed out that following embodiment is only
It is used to further illustrate the present invention, should not be understood as limiting the scope of the invention, which is skilled in technique
Personnel can make some nonessential modifications and adaptations to the present invention according to foregoing invention content.
Embodiment 1
2 g chitosans are taken, 2 g ferric chloride hexahydrates are dissolved in 96 g deionized waters, the heating stirring 1 in 90 DEG C of water-baths
Chitosan/ferric chloride in aqueous solution can be obtained so that chitosan is completely dissolved in h, and the 10 of 20 ml are added dropwise in aqueous solution
The sodium hydrate aqueous solution of wt% is continuously generated chitosan/ferric hydroxide precipitate in solution, and chitosan/ferric hydroxide precipitate is used
Deionized water repeated flushing, then gained floccule is added to 30 ml 5 wt% glutaraldehyde solution in be crosslinked 2 at 30 DEG C
Products therefrom is dried 24 h, i.e. chitosan/iron hydroxide compound adsorbent by h in lyophilized preparation.
Embodiment 2
5.0 g chitosans are taken, 3.0 g ferric chloride hexahydrates are dissolved in 92 g deionized waters, heat and stir under 90 DEG C of water-baths
2 h are mixed, so that chitosan is completely dissolved, chitosan/ferric chloride in aqueous solution is prepared, the 5 of 80 ml are added dropwise in the solution
The sodium hydrate aqueous solution of wt% can be continuously generated chitosan/ferric hydroxide precipitate in solution, by chitosan/ferric hydroxide precipitate
With deionized water repeated flushing, then gained floccule is added in the glutaraldehyde solution of 50 ml10 wt% at 40 DEG C and is crosslinked
1.5 h, and products therefrom is dried into 24 h in freeze drier, chitosan/iron hydroxide compound adsorbent can be obtained.
Embodiment 3
3.0 g chitosans are taken, 2.0 g ferric chloride hexahydrates are dissolved in 95 g deionized waters, heat and stir under 90 DEG C of water-baths
Mix 1 h.So that chitosan is completely dissolved, chitosan/ferric chloride in aqueous solution is prepared, then 60 ml are added dropwise in the solution
5 wt% sodium hydrate aqueous solution, chitosan/ferric hydroxide precipitate can be continuously generated in solution, by chitosan/hydroxide
Iron precipitating deionized water repeated flushing, then gained floccule is added to 30 ml 10 wt% glutaraldehyde solution in 60 DEG C
1 h of lower crosslinking, and unreacted glutaraldehyde is removed with deionized water repeated flushing again, and by products therefrom in freeze drier
Dry 24 h, can be obtained chitosan/iron hydroxide compound adsorbent.
Embodiment 4
5.0 g chitosans are taken, 3.0 g ferric chloride hexahydrates are dissolved in 92 g deionized waters, heat and stir under 90 DEG C of water-baths
1.5 h are mixed, so that chitosan is completely dissolved, chitosan/ferric chloride in aqueous solution is prepared, 50 ml are added dropwise in the solution
10 wt% sodium hydrate aqueous solution, chitosan/ferric hydroxide precipitate can be continuously generated in solution, by chitosan/hydroxide
Iron precipitating deionized water repeated flushing, then gained floccule is added to 100 ml 5 wt% epichlorohydrin solution in 30 DEG C
2 h of lower crosslinking, and products therefrom is dried into 24 h in freeze drier, chitosan/iron hydroxide compound adsorbent can be obtained.
Embodiment 5
5.0 g chitosans are taken, 5.0 g ferric chloride hexahydrates are dissolved in 90 g deionized waters, heat and stir under 90 DEG C of water-baths
2 h are mixed, so that chitosan is completely dissolved, chitosan/ferric chloride in aqueous solution is prepared, is added dropwise 50 ml's in the solution
The sodium hydrate aqueous solution of 10 wt% can be continuously generated chitosan/ferric hydroxide precipitate in solution, by chitosan/iron hydroxide
Precipitating deionized water repeated flushing, then gained floccule is added to 50 ml 10 wt% epichlorohydrin solution at 60 DEG C
2 h are crosslinked, and products therefrom is dried into 24 h in freeze drier, chitosan/iron hydroxide compound adsorbent can be obtained.
1 chitosan of table/iron hydroxide compound adsorbent performance indicator
The above is only a preferred embodiment of the present invention, protection scope of the present invention is not limited merely to above-mentioned implementation
Example, all technical solutions belonged under thinking of the present invention all belong to the scope of protection of the present invention.It should be pointed out that for the art
Those of ordinary skill for, several improvements and modifications without departing from the principles of the present invention, these improvements and modifications
It should be regarded as protection scope of the present invention.
Claims (1)
1. a kind of chitosan of arsenic-adsorbing/iron hydroxide compound adsorbent preparation method, which is characterized in that 5.0 g six hydration
Iron chloride is dissolved in 90 g deionized waters, takes 5.0 g chitosans, 2 h of heating stirring under 90 DEG C of water-baths, so that chitosan is complete
Chitosan/ferric chloride in aqueous solution is prepared in ferric chloride solution in fully dissolved, and the 10 of 50 ml are added dropwise in the solution
The sodium hydrate aqueous solution of wt% can be continuously generated chitosan/ferric hydroxide precipitate in solution, by chitosan/ferric hydroxide precipitate
With deionized water repeated flushing, then gained floccule is added to 50 ml 10 wt% epichlorohydrin solution in be crosslinked at 60 DEG C
2 h, and products therefrom is dried into 24 h in freeze drier, chitosan/iron hydroxide compound adsorbent can be obtained.
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| CN201610850199.6A CN106311163B (en) | 2016-09-27 | 2016-09-27 | A kind of preparation method of the chitosan of arsenic-adsorbing/iron hydroxide compound adsorbent |
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| CN201610850199.6A CN106311163B (en) | 2016-09-27 | 2016-09-27 | A kind of preparation method of the chitosan of arsenic-adsorbing/iron hydroxide compound adsorbent |
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| CN106311163B true CN106311163B (en) | 2019-06-07 |
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Families Citing this family (5)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN106853362B (en) * | 2017-01-11 | 2019-04-02 | 福州大学 | A kind of chitosan/aluminium hydroxide compound adsorbent preparation method for adsorbing fluorine |
| CN107282023B (en) * | 2017-08-25 | 2020-05-19 | 益阳医学高等专科学校 | Nano adsorbent for chemical waste liquid treatment and preparation method thereof |
| CN107413318B (en) * | 2017-09-01 | 2020-09-11 | 浙江致远环境科技有限公司 | Efficient nano adsorbent for industrial waste liquid treatment and preparation method thereof |
| CN110498998B (en) * | 2019-08-27 | 2021-12-24 | 宁波坚锋新材料有限公司 | Electromagnetic shielding engineering plastic with three-dimensional structure and preparation method thereof |
| CN115138339A (en) * | 2022-07-25 | 2022-10-04 | 贵州省地质矿产勘查开发局一0五地质大队 | Montmorillonite-chitosan-hydroxyl iron composite material and preparation method thereof |
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Patent Citations (4)
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| CN101623623A (en) * | 2009-07-28 | 2010-01-13 | 山东大学 | Method for preparing chitosan-ferric oxide composite absorption arsenic removal material |
| CN102641720A (en) * | 2012-04-01 | 2012-08-22 | 华南师范大学 | Preparation method for modified kieselguhr composite adsorbing material |
| CN104069831A (en) * | 2014-07-24 | 2014-10-01 | 中国地质大学（北京） | Efficient nitrate-removing granular absorbent and preparation method thereof |
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Non-Patent Citations (2)
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