CN107042095B - A kind of preparation method and application of chitosan-ferrotitanium compound compound adsorbent - Google Patents
A kind of preparation method and application of chitosan-ferrotitanium compound compound adsorbent Download PDFInfo
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- CN107042095B CN107042095B CN201710461690.4A CN201710461690A CN107042095B CN 107042095 B CN107042095 B CN 107042095B CN 201710461690 A CN201710461690 A CN 201710461690A CN 107042095 B CN107042095 B CN 107042095B
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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
- B01J20/0203—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising compounds of metals not provided for in B01J20/04
- B01J20/0211—Compounds of Ti, Zr, Hf
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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
- B01J20/0203—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising compounds of metals not provided for in B01J20/04
- B01J20/0225—Compounds of Fe, Ru, Os, Co, Rh, Ir, Ni, Pd, Pt
- B01J20/0229—Compounds of Fe
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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
- B01J20/28014—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
- B01J20/28019—Spherical, ellipsoidal or cylindrical
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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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- 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
- B01J2220/46—Materials comprising a mixture of inorganic and organic materials
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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
- C02F2101/20—Heavy metals or heavy metal compounds
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Abstract
A kind of preparation method and application of chitosan-ferrotitanium compound compound adsorbent, belongs to technical field of absorbent.The specific steps of which are as follows: the preparation of (1) ferrotitanium compound；(2) preparation of composite material microballoon；Use isopropyl titanate and green vitriol for raw material in step (1), isopropyl titanate is added in organic solvent, it stirs to even rear addition green vitriol, the solution being uniformly dissolved is added rapidly in the mixed solution of acetone-water, it stirs uniform and stable to precipitating, stand, by after washing of precipitate through being dried under vacuum to constant weight；Ferrotitanium compound obtained in step (1) is added in chitosan-acetic acid solution, is added drop-wise in sodium hydroxide solution after mixing evenly, is washed, chitosan-ferrotitanium compound complex microsphere is obtained after freeze-drying.The microballoon absorption particle of this method preparation has that easily separated, adsorption capacity is high, reusable characteristic, can be used as a kind of novel adsorbent and is applied in engineering of water treatment.
Description
Technical field
The present invention relates to a kind of chitosan-ferrotitanium compound complex microsphere adsorbent preparation method and applications, belong to suction
Attached dose of technical field.
Background technique
As modern industry is quick and high development, environmental pollution is getting worse for bring therewith, wherein water environment
Pollution problem it is even more more prominent.It is a large amount of due to the industries waste water such as modern industry traditional Chinese medicine, metallurgy, chemical industry, printing and dyeing, machinery
Discharge, causes the content of beary metal in Different Waters increasingly to increase.Heavy metal enters after environment by long-term accumulated, then passes through food
Object chain is enriched in vivo, this will cause extremely serious threat to biology and human health.Therefore, the weight in water removal is removed
Metal has very important significance to guarantee human health.
Chitosan can be used as the pregnant solution of metal ion, can be effectively removed heavy metal toxic in industrial wastewater from
Son.Adsorbent of the chitosan and its derivative as a kind of natural macromolecular material, because its is from a wealth of sources, nontoxic, degradable, easy
The features such as recycling, obtains paying much attention to and study extensively, have developed rapidly in water treatment field.But chitosan material has surface area
The small, disadvantages such as porosity is low, need to study and improve.
By studying the various nanometer materials with specific morphology and structure to toxic ion in drinking water or waste water or organic
Pollutant removal, Fe, the compound nano-material of Ti class have cheap, abundant raw material, environmental-friendly equal spies
Property, therefore, the present invention uses temperate condition, and organic polymer-inorganic composite materials are realized that the compound shell of preparing of molecular level gathers
Sugar-ferrotitanium compound complex microsphere, this material improves the surface area of chitosan and ion exchange capacities, in engineering of water treatment
In, it can be used as a kind of safe and efficient heavy metal absorbent
Summary of the invention
The present invention provides a kind of safe and efficient, environmental-friendly three-dimensional polymer chitosan-ferrotitanium compound complex microsphere
Preparation method and application.
The three-dimensional polymer chitosan that the present invention synthesizes-ferrotitanium compound complex microsphere have it is easily separated, adsorption capacity is high,
Reusable excellent performance.
Offer of the present invention prepares chitosan-ferrotitanium compound complex microsphere method, includes the following steps:
(1) preparation of ferrotitanium compound:
Isopropyl titanate and lauryl amine are dissolved in ethylene glycol solvent, green vitriol is added after stirring 6-10h, is stirred
To dissolution, solution A is obtained；By water and acetone by volume 1:60-1:70 be uniformly mixed obtain solution B；Solution is added in solution A
Continue in B stir 3-6h after, be centrifugally separating to obtain solid product, with ethanol washing for several times after, 40~90 DEG C of vacuum drying 8-
12h obtains ferrotitanium compound；
(2) preparation of composite material microballoon:
It dissolves chitosan in the aqueous acetic acid that mass percent concentration is 0.1%-1%, step (1) then is added
In ferrotitanium compound obtained, continue stir 1-3h after obtain solution D；Solution D, which is added dropwise to mass percent concentration, is
In the sodium hydroxide solution of 0.5%-2%, spherical particle (preferably diameter is 2-4mm) is obtained, then distills spherical particle
Water washs repeatedly be neutral to pH after, after 30-40 DEG C of drying, then be freeze-dried 12~obtain chitosan-ferrotitanium compound for 24 hours and is compound
Material microballoon.
The molar ratio of isopropyl titanate and green vitriol is 5:1-2:1 in above-mentioned steps (1)；Isopropyl titanate and 12
The molar ratio of amine is preferably 7:1-5:1.
The volume ratio of isopropyl titanate and ethylene glycol is 1:30-1:50 in above-mentioned steps (1)；Ethylene glycol and solution B volume ratio
For 1:2-1:3.
The concentration in aqueous acetic acid of chitosan described in above-mentioned steps (2) is 15~25g/L；Ferrotitanium compound and shell are poly-
The mass ratio of sugar is 1:1-1:6；Solution D and the volume ratio of sodium hydroxide solution are preferably 1:1-1:2.
The chitosan that the present invention obtains-ferrotitanium compound complex microsphere main structure is supported by chitosan and is in netted knot
Structure, spherical ferrotitanium compound microballoon is relatively uniform to be dispersed in inside chitosan, and FeTi nanoparticle average diameter is about
500-600nm。
Heavy metal in chitosan-ferrotitanium compound complex microsphere adsorbent adsorbed water body is utilized the present invention provides a kind of
Using preferably, the heavy metal ion includes lead ion, cadmium ion or copper ion.
Compared with prior art, chitosan prepared by the present invention-ferrotitanium compound complex microsphere adsorbent has following product
Pole effect:
The present invention is compound using bioabsorbable polymer material chitosan and ferrotitanium compound, and being prepared has three-dimensional core-shell structure copolymer
Following both sides optimization may be implemented in the chitosan of structure-ferrotitanium compound complex microsphere adsorbent.On the one hand, using shell
Glycan is substrate, realizes the efficient utilization of cheap biomaterial, is easily isolated, avoids the secondary pollution to environment；It is another
Aspect, chitosan and ferrotitanium compound it is compound after, formed three-dimensional porous structure, improve the specific surface area of adsorbent, increase
Effective efficiency group, to increase adsorbent to the adsorption capacity of heavy metal.
Detailed description of the invention
Fig. 1 is chitosan-ferrotitanium compound complex microsphere electron microscope；
Fig. 2 is adsorption capacity figure of the chitosan-ferrotitanium compound complex microsphere to lead ion.
Specific embodiment
The specific embodiment of preparation method and application of the present invention is provided below
Embodiment 1
(1) it takes 2ml isopropyl titanate and 0.185g lauryl amine to be dissolved in 80ml ethylene glycol, seven water of 0.46g is added after stirring 8h
Ferrous sulfate is closed, continues stirring to its dissolution, obtains solution A.Then it measures 170ml acetone and 2.7ml water is uniformly mixed and obtains
Solution A is poured into B and after stirring 3h, is centrifugally separating to obtain solid product by solution B, and for several times with ethanol washing, 40~90 DEG C true
The dry 8-12h of sky, obtains ferrotitanium compound；
(2) it takes 1.2g chitosan to be dissolved in the aqueous acetic acid of 60ml 1%, after stirring for 24 hours, 0.2g ferrotitanium is added
Object is closed, continues to be added dropwise in the sodium hydroxide solution that 100ml concentration is 1% after stirring 2h, obtains spherical that diameter is 2-4mm
Grain, then spherical particle is washed repeatedly with distilled water after being neutrality to pH, be freeze-dried again after 30 DEG C of drying 12h obtain shell gather
Sugar-ferrotitanium compound complex microsphere.
Absorption property test: Pb (NO is used3)2As toxic ion presoma, the lead ion that preparation obtains various concentration is molten
Liquid, concentration are respectively 10,20,50,100 and 200mgL-1.The Pb of various concentration 20mL is measured respectively2+Aqueous solution, then
20mg chitosan-ferrotitanium compound complex microsphere will be added thereto.After stirring 12h at room temperature, solid-liquid point is carried out to mixed liquor
From collection clear liquid.Using Pb in inductively coupled plasma atomic emission spectrum detection solution2+Concentration.According to absorption front and back weight
Metal ion solubility is poor, calculate adsorbent to Pb2+Maximal absorptive capacity be 17.8mg/g.
Embodiment 2
With embodiment 1, but in step (2), ferrotitanium additive amount is 0.4g to specific preparation process.
Absorption property test process is the same as embodiment 1.The adsorbent is to the maximal absorptive capacity of lead ion in corresponding solution
35.6mg/g。
Embodiment 3
With embodiment 1, but in step (2), ferrotitanium additive amount is 0.6g to specific preparation process.
Sem test: being scanned Electronic Speculum test for the chitosan of above-mentioned preparation-ferrotitanium compound complex microsphere,
Test results are shown in figure 1.
Fig. 1 shows chitosan-ferrotitanium compound complex microsphere particle that ferrotitanium additive amount is 0.6g in the present embodiment
Scanning electron microscope (SEM) photograph, as can be seen from the figure chitosan-ferrotitanium compound complex microsphere main structure is supported by chitosan and is in net
Shape structure, spherical ferrotitanium compound microballoon is relatively uniform to be dispersed in inside chitosan, and FeTi nanoparticle average diameter is about
For 400-500nm.
Absorption property test process is the same as embodiment 1.The adsorbent is to the maximal absorptive capacity of lead ion in corresponding solution
42.3mg/g。
Embodiment 4
With embodiment 1, but in step (2), ferrotitanium additive amount is 0.8g to specific preparation process.
Absorption property test process is the same as embodiment 1.The adsorbent is to the maximal absorptive capacity of lead ion in corresponding solution
66.4mg/g。
Claims (7)
1. a kind of prepare chitosan-ferrotitanium compound complex microsphere method, which comprises the steps of:
(1) preparation of ferrotitanium compound:
Isopropyl titanate and lauryl amine are dissolved in ethylene glycol solvent, green vitriol is added after stirring 6-10h, stirs to molten
Solution, obtains solution A；By water and acetone by volume 1:60-1:70 be uniformly mixed obtain solution B；Solution A is added in solution B
Continue stir 3-6h after, be centrifugally separating to obtain solid product, with ethanol washing for several times after, 40~90 DEG C of vacuum drying 8-12h are obtained
To ferrotitanium compound；
(2) preparation of composite material microballoon:
It dissolves chitosan in the aqueous acetic acid that mass percent concentration is 0.1%-1%, system in step (1) is then added
The ferrotitanium compound obtained continues to obtain solution D after stirring 1-3h；It is 0.5%-2% that solution D, which is added dropwise to mass percent concentration,
Sodium hydroxide solution in, obtain spherical particle, then wash spherical particle repeatedly with distilled water after being neutrality to pH, 30-
After 40 DEG C of dryings, then be freeze-dried 12~for 24 hours chitosan-ferrotitanium compound composite material microballoon.
2. a kind of chitosan-ferrotitanium compound complex microsphere method is prepared described in accordance with the claim 1, which is characterized in that
The molar ratio of isopropyl titanate described in step (1) and green vitriol is 5:1-2:1；Mole of isopropyl titanate and lauryl amine
Than for 7:1-5:1.
3. a kind of chitosan-ferrotitanium compound complex microsphere method is prepared described in accordance with the claim 1, which is characterized in that
The volume ratio of isopropyl titanate described in step (1) and ethylene glycol is 1:30-1:50；The volume ratio of ethylene glycol and solution B is 1:2-
1:3。
4. a kind of chitosan-ferrotitanium compound complex microsphere method is prepared described in accordance with the claim 1, which is characterized in that
The concentration in aqueous acetic acid of chitosan described in step (2) is 15~25g/L；The mass ratio of ferrotitanium compound and chitosan is
1:1-1:6。
5. a kind of chitosan-ferrotitanium compound complex microsphere method is prepared described in accordance with the claim 1, which is characterized in that
Solution D and the volume ratio of sodium hydroxide solution are 1:1-1:2 in step (2).
6. a kind of chitosan-ferrotitanium compound complex microsphere method is prepared described in accordance with the claim 1, which is characterized in that
Chitosan-ferrotitanium compound complex microsphere main structure is supported by chitosan and is in reticular structure, and spherical ferrotitanium compound is micro-
Ball is relatively uniform to be dispersed in inside chitosan, and FeTi nanoparticle average diameter is 400-500nm.
7. the chitosan that any one of claim 1-6 method is prepared-ferrotitanium compound complex microsphere application, at water
In reason, for adsorbing at least one of heavy metal ion lead ion, cadmium ion, copper ion ion.
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| CN108499541B (en) * | 2018-04-08 | 2019-10-18 | 山东建筑大学 | A kind of titanium sulfate-chitosan compounding filter aid and preparation method thereof |
| CN109046267A (en) * | 2018-08-20 | 2018-12-21 | 广州市环境保护技术设备公司 | A kind of preparation method and applications of citric acid grafted chitosan bead |
| CN112479392B (en) * | 2020-11-23 | 2021-08-27 | 纳琦绿能工程有限公司 | Composite sewage treatment agent and preparation method and application thereof |
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