CN108854986A - A kind of epoxychloropropane modified chitosan and preparation method thereof for adsorbing heavy metal ion - Google Patents
A kind of epoxychloropropane modified chitosan and preparation method thereof for adsorbing heavy metal ion Download PDFInfo
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- CN108854986A CN108854986A CN201810699066.2A CN201810699066A CN108854986A CN 108854986 A CN108854986 A CN 108854986A CN 201810699066 A CN201810699066 A CN 201810699066A CN 108854986 A CN108854986 A CN 108854986A
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- chitosan
- epoxychloropropane
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- heavy metal
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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
- B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
- B01J20/28054—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 surface properties or porosity
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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
- C02F2101/20—Heavy metals or heavy metal compounds
Abstract
The invention belongs to chitin modified technical fields, provide a kind of epoxychloropropane modified chitosan and preparation method thereof for adsorbing heavy metal ion.The preparation method includes：Acetic acid solution, chitosan, epoxychloropropane and NaOH solution are added hybrid reaction according to a certain percentage.Design is scientific and reasonable for the preparation method, easy to operate, and the epoxychloropropane modified chitosan with excellent absorption property can be prepared, and is suitable for industrialization large-scale production.Epoxychloropropane modified chitosan prepared by the above method, heavy metal ion adsorbed aspect of the epoxychloropropane modified chitosan in depollution waste water have the effect of excellent；Mechanical performance and stability are high, and pH value is applied widely in the solution, stronger to the absorption property absorption and selection performance of metal ion.
Description
Technical field
The invention belongs to chitin modified technical fields, specifically, being related to a kind of for adsorbing the ring of heavy metal ion
Oxygen chloropropane modification of chitosan and preparation method thereof.
Background technique
Today's society industrialization development is more and more flourishing, but also brings many harm, Jin Erwei to our environment simultaneously
Coerce the mankind.Especially industrialization development causes various heavy metal ion to flow into our water resource, invades ours
Soil.The processing of heavy metal ion has been to be concerned by more and more people now.Just at present handle water in heavy metal from
What sub- longest used has chemical method and physical method.
However, chemical method mainly includes electrolysis method and the precipitation method；Wherein, electrolysis method is only applicable to concentration higher concentration
In water, and the effect of low concentration is with regard to very poor；The precipitation method by precipitating reagent and environment because influenced, often except water concentration is not achieved
It is required that while being likely to cause secondary pollution.Physical method there is adsorption effects poor, higher cost, and active material
Regeneration rate is very low, is unsuitable for using on a large scale；Solution is lost in solution extraction process and extract liquor regenerative process will consume greatly
Energy, making this method, there are many deficiencies, therefore are much limited.
Summary of the invention
For deficiency above-mentioned in the prior art, the first object of the present invention is the provision of a kind of for adsorbing heavy metal
The epoxychloropropane modified chitosan of ion；Heavy metal ion of the epoxychloropropane modified chitosan in depollution waste water is inhaled
Subsidiary formula face has the effect of excellent；Mechanical performance and stability are high, and pH value is applied widely in the solution, to metal from
The absorption property absorption of son and selection performance are stronger.
For deficiency above-mentioned in the prior art, the second object of the present invention is the provision of a kind of for adsorbing heavy metal
The preparation method of the epoxychloropropane modified chitosan of ion；Design is scientific and reasonable for the preparation method, easy to operate, can prepare
The epoxychloropropane modified chitosan for the absorption property for having excellent is obtained, industrialization large-scale production is suitable for.
In order to achieve the above object, the solution that the present invention uses is：
It is a kind of for adsorbing the preparation method of the epoxychloropropane modified chitosan of heavy metal ion, including：In 48-52
Under the conditions of DEG C, chitosan to chitosan is added in 3% acetic acid solution and is completely dissolved, chitosan solution is formed；It is molten to chitosan
Epoxychloropropane is added dropwise in liquid, forms mixed solution；After reacting 30min, to the NaOH solution of mixed solution and dripping 5%, drop
When adding to the generation of no white precipitate, it is cooled to 20-30 DEG C, is first washed with distilled water and filters afterwards twice, then twice with acetone washing,
It is dry after suction filtration；Acetic acid solution, chitosan, epoxychloropropane and NaOH solution adding proportion be 100ml:0.51-
0.52g:2.8-3.2ml:24-26ml。
It is a kind of for adsorbing the epoxychloropropane modified chitosan of heavy metal ion, by above-mentioned for adsorbing heavy metal ion
The preparation method of epoxychloropropane modified chitosan be prepared.
A kind of epoxychloropropane modified chitosan and preparation method thereof for adsorbing heavy metal ion provided by the invention
Beneficial effect be：
(1) chitosan and epoxychloropropane are modified by the present invention under alkaline condition, obtain a kind of more micropores in surface,
The extremely strong polymer of adsorption effect.By creatively being compounded to each raw material according to certain proportion, can greatly improve
Mechanical performance and stability widen the scope of application of pH value in the solution, improve absorption and selection of the shell to metal ion
Performance.
(2) preparation method for the epoxychloropropane modified chitosan for adsorbing heavy metal ion that the present invention uses,
Preparation method is simple, and operation is easy, molten by using the acetic acid solution, chitosan, epoxychloropropane and the NaOH that centainly match
Liquid carries out compounding and the epoxychloropropane modified chitosan with excellent absorption property is prepared.
Detailed description of the invention
Fig. 1 is the adsorption effect comparison diagram of the 8 groups of adsorption experiments provided in experimental example 2.
Specific embodiment
It in order to make the object, technical scheme and advantages of the embodiment of the invention clearer, below will be in the embodiment of the present invention
Technical solution be clearly and completely described.The person that is not specified actual conditions in embodiment, according to normal conditions or manufacturer builds
The condition of view carries out.Reagents or instruments used without specified manufacturer is the conventional production that can be obtained by commercially available purchase
Product.
Below to provided in an embodiment of the present invention a kind of for adsorbing the epoxychloropropane modified chitosan of heavy metal ion
And preparation method thereof.
It is a kind of for adsorbing the preparation method of the epoxychloropropane modified chitosan of heavy metal ion, including：Using acetic acid
Solution, chitosan, epoxychloropropane and NaOH solution are 100ml according to adding proportion:0.51-0.52g:2.8-3.2ml:
24-26ml is compounded；Further, adding proportion 100ml:0.51-0.52g:3ml:25ml.
It should be noted that reaction principle is as follows in the present embodiment：Carbon chlorine key on epoxychloropropane is broken, and forms C+And the hydroxyl condensation in chitosan obtains ether；Hydroxyl in the epoxy addition of the other end and another chitosan at the same time
At ether, the chitosan with cross-linked structure is generated.Epoxychloropropane is reacted with chitosan crosslinked, not only increases chitosan itself
Mechanical performance, also accessed active group, changed activity.By controlling the point being crosslinked, make epoxychloropropane and shell poly-
- OH crosslinking on sugar backbone, thus can protect a large amount of-NH in chitosan molecule chain2, obtained product adsorption effect is also
To greatly improving.
Specifically, firstly, under the conditions of 48-52 DEG C, further under the conditions of 50 DEG C, 3% acetic acid solution is added
Chitosan to chitosan is completely dissolved, and forms chitosan solution.
It should be noted that in the present embodiment, using the temperature of heating water bath control reaction to keep in reaction process
It being capable of constant temperature.Specifically, in the present embodiment, it weighs chitosan in the balance to pour into three-necked bottle, and prepared 3% second is added
Acid solution；The devices such as iron stand, water-bath, constant speed stirrer are disposed, turn on agitator, speed is medium, by the control of water bath device
Temperature processed is tuned into 50 DEG C, controls temperature in reaction process at 48-52 DEG C, so that chitosan is completely molten under suitable conditions
Solution.
In the present embodiment, the configuration method of 3% acetic acid solution is as follows：It is fallen with the acetic acid solution that pipette measures 15ml
Enter in 500ml volumetric flask, then adds 485ml distilled water and be configured to the acetic acid solution that concentration is 3%, sufficiently shake up.
Then, epoxychloropropane is added dropwise into chitosan solution, forms mixed solution.Specifically, in the present embodiment, it uses
Pipette measures epoxychloropropane solution in separatory funnel, is slowly added dropwise into chitosan solution.It should be noted that
In the present embodiment, the time for adding of epoxychloropropane is 30min, to guarantee the speed being added dropwise, so that reaction be made to carry out ground more
Sufficiently.
Then, after dripping epoxychloropropane, 30min is reacted, then 5% NaOH solution is slowly added dropwise.
In the present embodiment, the configuration method of 5% NaOH solution is as follows：5gNaOH solid is weighed in the balance in small beaker
In, appropriate distilled water is added and is dissolved, is then transferred in 100ml large beaker, will be used to dissolve NaOH's with a small amount of distilled water
Solid small beaker washs three times, transfers in 100ml beaker, distilled water is added to 100ml graduation mark, is transferred to and uses rubber stopper
Narrow-mouthed bottle in, place.
After solution is added, white precipitate generation is had.When no white precipitate generates, it is cooled to 20-30 DEG C, first with steaming
Distilled water filters after washing twice, then twice with acetone washing, dry after suction filtration.In the present embodiment, the finished product after washing is put
It is placed in the thermostatic drying chamber that temperature is 60 DEG C and dries to constant weight.
Feature and performance of the invention are described in further detail with reference to embodiments.
Embodiment 1
The present embodiment provides a kind of for adsorbing the preparation method of the epoxychloropropane modified chitosan of heavy metal ion, wraps
It includes：
Under the conditions of 50 DEG C, the chitosan that 0.5008g is added in 3% acetic acid solution of 100ml is completely molten to chitosan
Solution forms chitosan solution；The epoxychloropropane of 3ml is added dropwise into chitosan solution, forms mixed solution；After reacting 30min,
It is cooled to 20-30 DEG C, is first used when being added dropwise to the generation of no white precipitate to 5% NaOH solution of mixed solution and dripping 25ml
Distilled water filters after washing twice, then twice with acetone washing, dry after suction filtration.
Embodiment 2
The present embodiment provides a kind of for adsorbing the preparation method of the epoxychloropropane modified chitosan of heavy metal ion, wraps
It includes：
Under the conditions of 50 DEG C, the chitosan that 0.5108g is added in 3% acetic acid solution of 100ml is completely molten to chitosan
Solution forms chitosan solution；The epoxychloropropane of 3ml is added dropwise into chitosan solution, forms mixed solution；After reacting 30min,
It is cooled to 20-30 DEG C, is first used when being added dropwise to the generation of no white precipitate to 5% NaOH solution of mixed solution and dripping 25ml
Distilled water filters after washing twice, then twice with acetone washing, dry after suction filtration.
Embodiment 3
The present embodiment provides a kind of for adsorbing the preparation method of the epoxychloropropane modified chitosan of heavy metal ion, wraps
It includes：
Under the conditions of 50 DEG C, the chitosan that 0.5102g is added in 3% acetic acid solution of 100ml is completely molten to chitosan
Solution forms chitosan solution；The epoxychloropropane of 3ml is added dropwise into chitosan solution, forms mixed solution；After reacting 30min,
It is cooled to 20-30 DEG C, is first used when being added dropwise to the generation of no white precipitate to 5% NaOH solution of mixed solution and dripping 25ml
Distilled water filters after washing twice, then twice with acetone washing, dry after suction filtration.
Embodiment 4
The present embodiment provides a kind of for adsorbing the preparation method of the epoxychloropropane modified chitosan of heavy metal ion, wraps
It includes：
Under the conditions of 50 DEG C, the chitosan that 0.5101g is added in 3% acetic acid solution of 100ml is completely molten to chitosan
Solution forms chitosan solution；The epoxychloropropane of 3ml is added dropwise into chitosan solution, forms mixed solution；After reacting 30min,
It is cooled to 20-30 DEG C, is first used when being added dropwise to the generation of no white precipitate to 5% NaOH solution of mixed solution and dripping 25ml
Distilled water filters after washing twice, then twice with acetone washing, dry after suction filtration.
Embodiment 5
The present embodiment provides a kind of for adsorbing the preparation method of the epoxychloropropane modified chitosan of heavy metal ion, wraps
It includes：
Under the conditions of 50 DEG C, the chitosan that 0.5006g is added in 3% acetic acid solution of 100ml is completely molten to chitosan
Solution forms chitosan solution；The epoxychloropropane of 3ml is added dropwise into chitosan solution, forms mixed solution；After reacting 30min,
It is cooled to 20-30 DEG C, is first used when being added dropwise to the generation of no white precipitate to 5% NaOH solution of mixed solution and dripping 25ml
Distilled water filters after washing twice, then twice with acetone washing, dry after suction filtration.
Embodiment 6
The present embodiment provides a kind of for adsorbing the preparation method of the epoxychloropropane modified chitosan of heavy metal ion, wraps
It includes：
Under the conditions of 50 DEG C, the chitosan that 0.5105g is added in 3% acetic acid solution of 100ml is completely molten to chitosan
Solution forms chitosan solution；The epoxychloropropane of 3ml is added dropwise into chitosan solution, forms mixed solution；After reacting 30min,
It is cooled to 20-30 DEG C, is first used when being added dropwise to the generation of no white precipitate to 5% NaOH solution of mixed solution and dripping 25ml
Distilled water filters after washing twice, then twice with acetone washing, dry after suction filtration.
Embodiment 7
The present embodiment provides a kind of for adsorbing the preparation method of the epoxychloropropane modified chitosan of heavy metal ion, wraps
It includes：
Under the conditions of 50 DEG C, the chitosan that 0.5003g is added in 3% acetic acid solution of 100ml is completely molten to chitosan
Solution forms chitosan solution；The epoxychloropropane of 3ml is added dropwise into chitosan solution, forms mixed solution；After reacting 30min,
It is cooled to 20-30 DEG C, is first used when being added dropwise to the generation of no white precipitate to 5% NaOH solution of mixed solution and dripping 25ml
Distilled water filters after washing twice, then twice with acetone washing, dry after suction filtration.
Experimental example 1：The measurement of the degree of polymerization
Experimental method：The quality of the chitosan that measurement embodiment 1-7 is provided respectively before the reaction, is denoted as M1, then measure reality
The quality for testing the epoxychloropropane modified chitosan for adsorbing heavy metal ion that a 1-7 is provided, is denoted as M2, degree of cross linking Z
(%)=(M2-M1)/M1, the degree of cross linking of embodiment 1-7 are shown in Table 1：
The coefficient of softing of 1 experimental group 1-12 of table
| Group number | M1(g) | M2(g) | Z (%) |
| 1 | 0.5008 | 0.6751 | 34.80 |
| 2 | 0.5108 | 0.7012 | 37.27 |
| 3 | 0.5102 | 0.6801 | 33.30 |
| 4 | 0.5101 | 0.7008 | 37.38 |
| 5 | 0.5006 | 0.6812 | 36.08 |
| 6 | 0.5105 | 0.6634 | 29.95 |
| 7 | 0.5003 | 0.6684 | 33.60 |
According to 1 data of table it is found that the crosslinking degree of embodiment 1-7 is very good.During entire polymerization experiment, influence
The reason of degree of cross linking, has very much.There are internal factor and external factor.Internal factor is exactly the dosage of various substances when reacting, dosage
Number be the key that directly control the degree of cross linking, the especially proportion of both chitosan and epoxychloropropane.External factor has instead
The speed of seasonable temperature, stirring plus the speed of reactant etc., they are all affecting the degree of cross linking.The present invention is exactly inventor
Reasonable raw material proportioning, and the temperature of reaction are creatively used, the comprehensive functions such as the speed that raw material is added dropwise, ability are aided with
Access the excellent degree of cross linking.
Experimental example 2：Adsorption experiment
Experimental method：
(1) the 10 of 100ml is configured-4The Cu of mol/L2+Solution is poured into respectively in the beaker of 8 100ml, each beaker
Liquor capacity is 100ml, respectively number 1,2,3,4,5,6,7,8.
(2) crosslinking that 0.3486g chitosan and epoxychloropropane are separately added into the 100ml solution that number is 1-7 is poly-
Object is closed, No. 8 beakers are added without anything, are set as reference group.At the time 10,20,30,40,50,60,120,240 minutes
The measurement of absorbance is carried out with spectrophotometer.
Experimental data is as shown in Figure 1.According to Fig. 1 data, it can be clearly seen that after different time intervals, in solution
Absorption take the lead in reducing and increase again, but the absorptivity that finally reaches of 1-7 and the 8 obvious reduction of absorptivity illustrate in solution
Cu2+It is reducing.
In conclusion using provided by the present invention for adsorb heavy metal ion epoxychloropropane modified chitosan and its
Preparation method：Heavy metal ion adsorbed aspect of the epoxychloropropane modified chitosan in depollution waste water has excellent effect
Fruit；Mechanical performance and stability are high, and pH value is applied widely in the solution, to the absorption property absorption of metal ion with
Select performance stronger.Restructuring Preparation Method, design is scientific and reasonable, easy to operate, can be prepared with excellent absorption property
Epoxychloropropane modified chitosan is suitable for industrialization large-scale production.
The foregoing is only a preferred embodiment of the present invention, is not intended to restrict the invention, for the skill of this field
For art personnel, the invention may be variously modified and varied.All within the spirits and principles of the present invention, made any to repair
Change, equivalent replacement, improvement etc., should all be included in the protection scope of the present invention.
Claims (5)
1. a kind of for adsorbing the preparation method of the epoxychloropropane modified chitosan of heavy metal ion, it is characterised in that：Including：
Under the conditions of 48-52 DEG C, chitosan to the chitosan is added in 3% acetic acid solution and is completely dissolved, chitosan solution is formed；
Epoxychloropropane is added dropwise into the chitosan solution, forms mixed solution；After reacting 30min, dripped into the mixed solution
The NaOH solution for adding 5% is cooled to 20-30 DEG C, is first washed with distilled water and takes out afterwards twice when being added dropwise to the generation of no white precipitate
Filter, then twice with acetone washing, it is dry after suction filtration；The acetic acid solution, the chitosan, the epoxychloropropane and described
The adding proportion of NaOH solution is 100ml:0.51-0.52g:2.8-3.2ml:24-26ml.
2. it is according to claim 1 for adsorbing the preparation method of the epoxychloropropane modified chitosan of heavy metal ion,
It is characterized in that：The acetic acid solution, the chitosan, the epoxychloropropane and the NaOH solution adding proportion be
100ml:0.51-0.52g:3ml:25ml。
3. it is according to claim 1 for adsorbing the preparation method of the epoxychloropropane modified chitosan of heavy metal ion,
It is characterized in that：Using the temperature of heating water bath control reaction.
4. it is according to claim 1 for adsorbing the preparation method of the epoxychloropropane modified chitosan of heavy metal ion,
It is characterized in that：The time for adding of the epoxychloropropane is 30min.
5. a kind of for adsorbing the epoxychloropropane modified chitosan of heavy metal ion, it is characterised in that：As described in claim 1
The preparation method of the epoxychloropropane modified chitosan for adsorbing heavy metal ion be prepared.
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| CN112547020A (en) * | 2020-10-13 | 2021-03-26 | 黄淮学院 | Preparation method of chitosan-based composite material |
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