CN106622162A - Preparation method and application of modified chitosan/zeolite/nano-zirconium adsorbent - Google Patents
Preparation method and application of modified chitosan/zeolite/nano-zirconium adsorbent Download PDFInfo
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- CN106622162A CN106622162A CN201710034978.3A CN201710034978A CN106622162A CN 106622162 A CN106622162 A CN 106622162A CN 201710034978 A CN201710034978 A CN 201710034978A CN 106622162 A CN106622162 A CN 106622162A
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- zeolite
- chitosan
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- nanometer zirconium
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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
- C02F1/288—Treatment of water, waste water, or sewage by sorption using composite sorbents, e.g. coated, impregnated, multi-layered
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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
- C02F2101/16—Nitrogen compounds, e.g. ammonia
-
- 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
- C02F2101/16—Nitrogen compounds, e.g. ammonia
- C02F2101/163—Nitrates
Abstract
The invention belongs to the technical field of water treatment medicaments and particularly relates to a preparation method and application of a modified chitosan/zeolite/nano-zirconium adsorbent. The preparation method comprises the steps of firstly preparing a chitosan acetic acid solution, forming a Y-form zeolite/nano-ZrO2 mixture, adding the mixture into the chitosan acetic acid solution, heating at 50-55 DEG C in a drying box for 5-5.5 hours so as to form a modified chitosan/zeolite/nano-zirconium mixture, adding the modified chitosan/zeolite/nano-zirconium mixture into a glutaraldehyde solution so as to obtain a reactant, and washing and drying the reactant, so as to obtain the modified chitosan/zeolite/nano-zirconium adsorbent. The preparation method has the beneficial effects that the defect that a conventional water treatment medicament currently used in water plants has poor treatment effects to exceeding nitrate and ammonia nitrogen raw water is overcome, the preparation process is simple, the feeding is convenient, the recycling is realized, the influence of environmental factors is low, a water treatment structure does not need to be added, and thus the cost is saved.
Description
Technical field
The invention belongs to technical field of water treatment chemical, and in particular to a kind of modification of chitosan/zeolite/nanometer zirconium adsorbent
Preparation method and application.
Background technology
Due to widespread pollution from the overuse of fertilizers and pesticides in rural area and industrial pollution, cause to contain nitric acid in China's most area surface water and groundwater
The pollutant such as salt and ammonia nitrogen, according to《National urban drinking water safety ensures planning（2006-2020）》Data, the whole nation nearly 20%
The centralized groundwater source water quality in city be inferior to Group III, and nitrate, ammonia and nitrogen pollution are main problems.Especially China's agriculture
The main drinking water source of village's most area is underground water, and in underground water people is known from experience containing nitrate, ammonia and nitrogen pollution and produced
The larger harm of life, the breathing that nitrate passes through destruction cell and tissue causes lactic acid in blood, cholesterol and white blood cell to increase
Plus, protein is reduced in a large number, and so as to cause various diseases, and ammonia nitrogen easily can produce nitrite in processing procedure in water
Nitrogen, and nitrite nitrogen can produce carcinogenic nitrosamine with the protein of human body, and the water of nitrite nitrogen is drunk for a long time to human body
It is very harmful.China《Standards for drinking water quality》（GB5749-2006）Stricter wanting is proposed to nitrate, ammonia nitrogen
Ask, respectively provided the nitrate limit value with surface water as water source be 10mg/L, the nitrate limit value with underground water as water source be
20mg/L, the limit value of ammonia nitrogen are 0.5mg/L, and water treatment plant of China generally adopts common process, i.e. " coagulation-precipitate-filter-disappear
Poison ", the technique is poor for the removal ability of nitrate, ammonia nitrogen.At present, nitrate, ammonia and nitrogen pollution treatment technology mainly include
Ion-exchange, electroosmose process, chemical oxidization method, bioanalysis etc., but these methods it is relatively costly, by such environmental effects compared with
Greatly and it is easy to produce secondary pollution, therefore is not suitable for the application of drinking water treatment technology.
Shitosan（CTS）It is a kind of cationic polysaccharide, in being widely present in shellfish, due to containing in its molecular structure
There are substantial amounts of amino and hydroxyl isoreactivity group, property is more active, can modify, activates and be coupled, therefore variousization can occur
Learn modified, shitosan can be generated by acylation, N- alkylatings, Schiff effect, quaternization effect more
Kind of derivative, and can couple to form multifunctional composite with magnetic material, nano material, microorganism, coagulant etc., in water
Processing especially drinking water treatment field has quite wide application prospect.
The content of the invention
For there is the pollution problems such as nitrate, ammonia nitrogen in water, the present invention provides a kind of modification of chitosan/zeolite/nanometer
The preparation method and application of zirconium adsorbent, it is therefore an objective to which the existing conventional treatment process of solution is to nitrate, ammonia nitrogen removal energy in water
The poor problem of power.
The preparation method of the modification of chitosan/zeolite/nanometer zirconium adsorbent of the present invention is followed the steps below：
（1）In adding chitosan into the acetum that volume fraction is 0.8% ~ 1.2%, weight fraction 1.8% ~ 2.2% is configured to
Chitosan-acetic acid solution；
（2）By y-type zeolite and nanometer ZrO2According to mass ratio (2-3):1 mixing, forms y-type zeolite/nanometer ZrO2Mixture；
（3）By step（2）In mixture be added to step（1）In chitosan-acetic acid solution in, volume ratio is 1:（3-
5）, heating 5-5.5h in 50-55 DEG C of drying box is placed in after mixing, form modification of chitosan/zeolite/nanometer zirconium mixture；
（4）By step（3）In resulting modification of chitosan/zeolite/nanometer zirconium mixture, be added to volume fraction for 24.8% ~
In 25.2% glutaraldehyde solution, 1h is stirred in 58 DEG C ~ 62 DEG C, obtain product；
（5）Deionized water rinsing step（4）Product to washing lotion for neutrality, then in 58 DEG C ~ 62 DEG C of drying box do
Dry 12h, desciccate is crushed, and obtains modification of chitosan/zeolite/nanometer zirconium adsorbent.
Wherein, described deacetylating degree of chitosan >=85%.
The application of the modification of chitosan/zeolite/nanometer zirconium adsorbent of the present invention is followed the steps below：
During modification of chitosan/zeolite/nanometer zirconium adsorbent is put into containing nitrate, the water sample of ammonia nitrogen pollutant, the shell that is modified gathers
Sugar/zeolite/nanometer zirconium adsorbent dosage is 1.0-1.5g/L, and mixing time is 30-40min, and mixing speed is 80-100r/
Min, to the clearance of nitrate 57.5% ~ 70% is can reach, and the clearance of ammonia nitrogen reaches 77.5-85.6%, and range of reaction temperature is
10-30℃。
Wherein, nitrate pollutants content is 20-30mg/L in described water sample, and ammonia nitrogen pollutant content is 2-5mg/L.
Compared with prior art, of the invention the characteristics of and beneficial effect are：
（1）Modification of chitosan/zeolite/nanometer zirconium adsorbent water treatment agent prepared by the present invention, is using shitosan surface
Various active functional group and nitrate, ammonia nitrogen formed the alkali metal cation that contains in complex reaction, and y-type zeolite duct and
Hydrone forms exchange reaction with nitrate, ammonia nitrogen, and using shitosan/y-type zeolite and ZrO2The nanostructured for being formed,
The interstitial space and specific surface area of particle surface is increased, is conducive to the nitrate in particle and water, ammonia nitrogen to be fully contacted,
The physisorption of particle surface is improved, so as to compensate for conventional water treatment medicament that current water factory uses to exceeded nitric acid
The defect of salt, ammonia nitrogen original sub-block effect difference；
（2）Preparation process of the present invention is simple, adds conveniently, and recoverable is little by such environmental effects, without the need for increasing water process newly
Structures, it is cost-effective.
Description of the drawings
Fig. 1 is the scanning electron microscopic picture of the modification of chitosan/zeolite/nanometer zirconium adsorbent prepared in embodiment 1；
Fig. 2 is water outlet nitric acid after different nitrate concentration modification of chitosan/zeolite/nanometer zirconium sorbent treatments in embodiment 1-3
The comparison diagram of salinity and clearance；
Fig. 3 is that water outlet ammonia nitrogen is dense after different ammonia nitrogen concentration modification of chitosan/zeolite/nanometer zirconium sorbent treatments in embodiment 1-3
The comparison diagram of degree and clearance.
Specific embodiment
Following specific embodiments are that present invention is further illustrated, but the flesh and blood of the present invention and are not only limited
In described in following specific embodiments, any combination between any specific embodiment and the simple change to preparation process belong to
In protection domain of the presently claimed invention.
Embodiment 1
The preparation of the modification of chitosan/zeolite of the present embodiment/nanometer zirconium adsorbent is followed the steps below：
（1）The shitosan that deacetylation is 85% is added in the acetum that volume fraction is 0.8%, weight fraction is configured to
1.8% chitosan-acetic acid solution；
（2）By y-type zeolite and nanometer ZrO2According to mass ratio 2:1 mixing, forms y-type zeolite/nanometer ZrO2Mixture；
（3）By step（2）In mixture be added to step（1）In chitosan-acetic acid solution in, volume ratio is 1:3, mix
Heating 5h in 50 DEG C of drying boxes is placed in after conjunction, modification of chitosan/zeolite/nanometer zirconium mixture is formed；
（4）By step（3）In resulting modification of chitosan/zeolite/nanometer zirconium mixture, be added to volume fraction for 25.2%
Glutaraldehyde solution in, in 58 DEG C stir 1h, obtain product；
（5）Deionized water rinsing step（4）Product be neutrality to washing lotion, then be dried 12h in 58 DEG C of drying box,
Desciccate is crushed, powdered modified shitosan/zeolite/nanometer zirconium adsorbent is obtained.
By the powdered modified shitosan/zeolite of scanning electron microscopic observation/nanometer zirconium adsorbent surface structure, as shown in figure 1,
As can be seen from Figure 1 absorbent particles pore structure is more, and Pore Diameter Specific Surface product is big, by increasing capacitance it is possible to increase nitrate, ammonia nitrogen in water
Deng pollutant and intergranular contact area, the physisorption of particle surface is improve.
Modification of chitosan/the zeolite of the present embodiment/nanometer zirconium adsorbent remove nitrate, ammonia nitrogen pollutant application according to
Following steps are carried out：
During modification of chitosan/zeolite/nanometer zirconium adsorbent is put into containing nitrate, the water sample of ammonia nitrogen pollutant, the shell that is modified gathers
Sugar/zeolite/Nano-Zinc adsorbent dosage is 1.0g/L, and mixing time is 30min, and mixing speed is 80r/min, nitrate
Clearance can reach 57.5%, as shown in Fig. 2 the clearance of ammonia nitrogen reaches 77.5%, as shown in figure 3, reaction temperature is 10 DEG C.Its
In, nitrate pollutants content is 20mg/L in described water sample, and ammonia nitrogen pollutant content is 2.0mg/L.
Embodiment 2
The preparation of the modification of chitosan/zeolite of the present embodiment/nanometer zirconium adsorbent is followed the steps below：
（1）The shitosan that deacetylation is 90% is added in the acetum that volume fraction is 0.8%, weight fraction is configured to
2% chitosan-acetic acid solution；
（2）By y-type zeolite and nanometer ZrO2According to mass ratio 2:1 mixing, forms y-type zeolite/nanometer ZrO2Mixture；
（3）By step（2）In mixture be added to step（1）In chitosan-acetic acid solution in, volume ratio is 1:4, mix
Heating 5.5h in 55 DEG C of drying boxes is placed in after conjunction, modification of chitosan/zeolite/nanometer zirconium mixture is formed；
（4）By step（3）In resulting modification of chitosan/zeolite/nanometer zirconium mixture, be added to volume fraction for 24.8%
Glutaraldehyde solution in, in 60 DEG C stir 1h, obtain product；
（5）Deionized water rinsing step（4）Product be neutrality to washing lotion, then be dried 12h in 60 DEG C of drying box,
Desciccate is crushed, modification of chitosan/zeolite/nanometer zirconium adsorbent is obtained.
The present embodiment modification of chitosan/zeolite/nanometer zirconium adsorbent remove nitrate, ammonia nitrogen pollutant application according to
Lower step is carried out：
During modification of chitosan/zeolite/nanometer zirconium adsorbent is put into containing nitrate, the water sample of ammonia nitrogen pollutant, the shell that is modified gathers
Sugar/zeolite/nanometer zirconium adsorbent dosage is 1.2g/L, and mixing time is 30min, and mixing speed is 100r/min, nitrate
Clearance can reach 67.2%, as shown in Fig. 2 the clearance of ammonia nitrogen reaches 82.6%, as shown in figure 3, reaction temperature is 15 DEG C.
Wherein, nitrate pollutants content is 25mg/L in described water sample, and ammonia nitrogen pollutant content is 3mg/L.
Embodiment 3
The preparation of the modification of chitosan/zeolite of the present embodiment/nanometer zirconium adsorbent is followed the steps below：
（1）The shitosan that deacetylation is 90% is added in the acetum that volume fraction is 0.8%, weight fraction is configured to
2.2% chitosan-acetic acid solution；
（2）By y-type zeolite and nanometer ZrO2According to mass ratio 3:1 mixing, forms y-type zeolite/nanometer ZrO2Mixture；
（3）By step（2）In mixture be added to step（1）In chitosan-acetic acid solution in, volume ratio is 1:5, mix
Heating 5h in 50 DEG C of drying boxes is placed in after conjunction, modification of chitosan/zeolite/nanometer zirconium mixture is formed；
（4）By step（3）In resulting modification of chitosan/zeolite/nanometer zirconium mixture, it is 25% to be added to volume fraction
In glutaraldehyde solution, 1h is stirred in 62 DEG C, obtain product；
（5）Deionized water rinsing step（4）Product be neutrality to washing lotion, then be dried 12h in 62 DEG C of drying box,
Desciccate is crushed, modification of chitosan/zeolite/nanometer zirconium adsorbent is obtained.
Modification of chitosan/the zeolite of the present embodiment/nanometer zirconium adsorbent remove nitrate, ammonia nitrogen pollutant application according to
Following steps are carried out：
During modification of chitosan/zeolite/nanometer zirconium adsorbent is put into containing nitrate, the water sample of ammonia nitrogen pollutant, the shell that is modified gathers
Sugar/zeolite/nanometer zirconium adsorbent dosage is 1.5g/L, and mixing time is 40min, and mixing speed is 100r/min, nitrate
Clearance can reach 70%, as shown in Fig. 2 the clearance of ammonia nitrogen reaches 85.6%, as shown in figure 3, reaction temperature is 30 DEG C.Its
In, nitrate pollutants content is 30mg/L in described water sample, and ammonia nitrogen pollutant content is 5mg/L.
Claims (4)
1. the preparation method of a kind of modification of chitosan/zeolite/nanometer zirconium adsorbent, it is characterised in that follow the steps below：
（1）In adding chitosan into the acetum that volume fraction is 0.8% ~ 1.2%, weight fraction 1.8% ~ 2.2% is configured to
Chitosan-acetic acid solution；
（2）By y-type zeolite and nanometer ZrO2According to mass ratio (2-3):1 mixing, forms y-type zeolite/nanometer ZrO2Mixture；
（3）By step（2）In mixture be added to step（1）In chitosan-acetic acid solution in, volume ratio is 1:（3-
5）, heating 5-5.5h in 50-55 DEG C of drying box is placed in after mixing, form modification of chitosan/zeolite/nanometer zirconium mixture；
（4）By step（3）In resulting modification of chitosan/zeolite/nanometer zirconium mixture, be added to volume fraction for 24.8% ~
In 25.2% glutaraldehyde solution, 1h is stirred in 58 DEG C ~ 62 DEG C, obtain product；
（5）Deionized water rinsing step（4）Product to washing lotion for neutrality, then in 58 DEG C ~ 62 DEG C of drying box do
Dry 12h, desciccate is crushed, and obtains modification of chitosan/zeolite/nanometer zirconium adsorbent.
2. a kind of preparation method of modification of chitosan/zeolite/nanometer zirconium adsorbent according to claim 1, its feature exists
In described deacetylating degree of chitosan >=85%.
3. the application of a kind of modification of chitosan/zeolite/nanometer zirconium adsorbent as claimed in claim 1, it is characterised in that according to
Following steps are carried out：
During modification of chitosan/zeolite/nanometer zirconium adsorbent is put into containing nitrate, the water sample of ammonia nitrogen pollutant, the shell that is modified gathers
Sugar/zeolite/nanometer zirconium adsorbent dosage is 1.0-1.5g/L, and mixing time is 30-40min, and mixing speed is 80-100r/
Min, to the clearance of nitrate 57.5% ~ 70% is can reach, and the clearance of ammonia nitrogen reaches 77.5-85.6%, and range of reaction temperature is
10-30℃。
4. a kind of application of modification of chitosan/zeolite/nanometer zirconium adsorbent according to claim 1, it is characterised in that institute
Nitrate pollutants content is 20-30mg/L in the water sample stated, and ammonia nitrogen pollutant content is 2-5mg/L.
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| CN110436680A (en) * | 2019-08-02 | 2019-11-12 | 吉林建筑大学 | A kind of processing method of nanoparticles to pharmaceutical wastewater |
| CN110665474A (en) * | 2019-10-30 | 2020-01-10 | 武汉工程大学 | Modified chitosan cross-linked zeolite porous adsorbent and application thereof |
| CN114950373A (en) * | 2022-05-30 | 2022-08-30 | 广西科技师范学院 | Preparation method and application of magnetic zirconium-loaded chitosan modified zeolite composite adsorbent |
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| CN114950373A (en) * | 2022-05-30 | 2022-08-30 | 广西科技师范学院 | Preparation method and application of magnetic zirconium-loaded chitosan modified zeolite composite adsorbent |
| CN114950373B (en) * | 2022-05-30 | 2023-12-29 | 广西科技师范学院 | Preparation method and application of magnetic zirconium-loaded chitosan modified zeolite composite adsorbent |
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