CN112892491A - Preparation method and application of edible chitosan-pectin gel beads for adsorbing heavy metals - Google Patents
Preparation method and application of edible chitosan-pectin gel beads for adsorbing heavy metals Download PDFInfo
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- CN112892491A CN112892491A CN202110075358.0A CN202110075358A CN112892491A CN 112892491 A CN112892491 A CN 112892491A CN 202110075358 A CN202110075358 A CN 202110075358A CN 112892491 A CN112892491 A CN 112892491A
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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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- 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
- B01J20/28021—Hollow particles, e.g. hollow spheres, microspheres or cenospheres
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- 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
- B01J20/28047—Gels
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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
- C02F1/285—Treatment of water, waste water, or sewage by sorption using synthetic organic 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
- 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 preparation method of edible chitosan-pectin gel beads for adsorbing heavy metals, which comprises the following steps: step 1, preparing chitosan-pectin hydrosol: dissolving chitosan and pectin in hydrochloric acid solution, and stirring to obtain chitosan-pectin hydrosol; step 2, preparing chitosan-pectin wet gel balls: slowly dripping the chitosan-pectin hydrosol prepared in the step 1 into caustic soda flake solution drop by drop to prepare chitosan-pectin wet gel balls; step 3, preparing chitosan-pectin gel beads: and (3) washing the chitosan-pectin wet gel balls prepared in the step (2) with distilled water to be neutral, and then carrying out freeze drying to prepare the edible chitosan-pectin gel beads capable of adsorbing heavy metals. The chitosan-pectin gel beads prepared by the method have the advantages of good stability, high mechanical strength, excellent adsorption performance and the like, do not need a chemical cross-linking agent in the preparation process, and are green and safe.
Description
Technical Field
The invention belongs to the technical field of preparation of water treatment materials, and particularly relates to a preparation method and application of edible chitosan-pectin gel beads for adsorbing heavy metals.
Background
With the rapid development of modernization, urbanization and industrialization, the heavy metal pollution problem is increasingly prominent. Heavy metals such as lead, copper, cadmium, mercury, etc., are difficult to biodegrade, have strong toxicity at low exposure levels, and can be accumulated in organisms through food chains to harm human life and health.
At present, common methods for removing heavy metals include chemical precipitation, ion exchange, electrochemical reaction, adsorption and the like, wherein adsorption is one of the most economical and effective methods. However, the current adsorbents for adsorbing and removing heavy metals have the main disadvantages: the preparation process of the adsorbent is complex, the adsorbent is not green enough, and the secondary pollution phenomenon exists, especially in the treatment of drinking water, fruit juice, beverage and the like closely related to human life. Therefore, there is a need for a novel edible adsorbent having a simple preparation process, being green and safe, causing no secondary pollution, and having excellent adsorption properties.
Chitosan is an environment-friendly basic polysaccharide, has the characteristics of biodegradability, low price, environmental protection and the like, contains rich functional groups (such as amino, carboxyl, hydroxyl and the like) capable of being combined with heavy metals, and is considered to be one of the most promising biological adsorbents. However, chitosan has the disadvantages of instability in acidic solutions, poor mechanical strength, low adsorption capacity, etc., which have hindered its application in the field of heavy metal removal. Common modification methods are complicated, and most use chemical cross-linking agents with extremely high toxicity. Therefore, the edible chitosan-pectin gel beads with good stability, high mechanical strength and excellent adsorption performance are prepared by a green and safe method without adopting a chemical cross-linking agent, heavy metals in a water sample are adsorbed and removed, and the method has a good market application prospect.
Disclosure of Invention
The invention aims to provide a preparation method of edible chitosan-pectin gel beads for adsorbing heavy metals, and the preparation process of the gel beads does not need to adopt a chemical cross-linking agent, is green and safe, and has the advantages of good stability, high mechanical strength, excellent adsorption performance and the like.
In order to achieve the purpose, the invention adopts the following technical scheme:
step 1, preparing chitosan-pectin hydrosol: dissolving chitosan and pectin in hydrochloric acid solution, and stirring to obtain chitosan-pectin hydrosol; wherein pectin is used as a natural crosslinking component, which can improve the stability, mechanical strength and adsorption performance of the chitosan-pectin gel beads.
Step 2, preparing chitosan-pectin wet gel balls: slowly dripping the chitosan-pectin hydrosol prepared in the step 1 into caustic soda flake solution drop by drop to prepare chitosan-pectin wet gel balls; the chitosan-pectin wet gel balls obtained at the moment are light yellow wet gel balls; the chitosan-pectin hydrosol prepared in the step 1 is insoluble in an alkali solution, so that a complete sphere can be formed by dropping the chitosan-pectin hydrosol into the alkali solution.
Step 3, preparing chitosan-pectin gel beads: washing the chitosan-pectin wet gel balls prepared in the step 2 to be neutral by using distilled water, and then carrying out freeze drying to prepare the edible chitosan-pectin gel beads capable of adsorbing heavy metals.
Freeze drying is adopted, firstly, the drying is because the dried chitosan-pectin gel beads are easy to store and convenient to use; and secondly, adopting freeze drying to control the porous structure of the chitosan-pectin wet gel spheres to obtain the chitosan-pectin gel beads with small pore diameter and large specific surface area.
Preferably, in the step 1, the mass concentration of the chitosan is 0.01g/mL to 0.05g/mL, and the mass concentration of the pectin is 0.01g/mL to 0.05 g/mL.
Preferably, the hydrochloric acid solution in the step 1 is a food grade hydrochloric acid solution, and the pH value of the hydrochloric acid solution is 1 to 2.
Preferably, the caustic soda flake solution in the step 2 is a food-grade caustic soda flake solution, and the concentration of the caustic soda flake solution is 1mol/L to 2 mol/L.
Preferably, in the step 3, the temperature of freeze drying is-80 ℃ to-50 ℃, and the time of freeze drying is 24h to 48 h.
The invention also provides application of the chitosan-pectin gel beads, namely the chitosan-pectin gel beads are used for adsorbing heavy metal ions in a water sample.
Preferably, the heavy metal ions include: cu2+、Cd2+、Hg2+And Pb2+。
The invention has the advantages that:
1. the edible chitosan-pectin gel beads are prepared, and no chemical cross-linking agent is needed in the preparation process, so that the edible chitosan-pectin gel beads are green and safe.
2. The prepared edible chitosan-pectin gel beads adopt pectin as a natural crosslinking component, improve the stability, mechanical strength and adsorption performance of the adsorbent, and can be used for adsorbing and removing heavy metals in a water sample.
Drawings
FIG. 1 is a scanning electron microscope photograph of chitosan-pectin gel beads
FIG. 2 shows N of chitosan-pectin gel beads2Adsorption and desorption (inset: chitosan-pectin gel bead pore size distribution diagram).
Detailed Description
For a better understanding of the present invention, reference will now be made to the following examples which are set forth to illustrate, but are not to be construed to limit the present invention.
Example 1
Adsorb Cu2+The preparation of the edible chitosan-pectin gel beads comprises the following steps:
step 1, preparing chitosan-pectin hydrosol: dissolving 2g of chitosan and 1g of pectin in 100mL of food-grade hydrochloric acid solution with the acidity value of 1, and uniformly stirring at room temperature to prepare chitosan-pectin hydrosol;
step 2, preparing chitosan-pectin wet gel balls: slowly dripping the chitosan-pectin hydrosol prepared in the step 1 into 1mol/L edible caustic soda flakes solution drop by drop to obtain light yellow chitosan-pectin wet gel balls;
step 3, preparing chitosan-pectin gel beads: washing the chitosan-pectin wet gel balls prepared in the step 2 with distilled water to be neutral, and then placing the gel balls in a freeze dryer (FD-IC vacuum freeze dryer, Telstar company, Spain) (-50 ℃, 48h) for freeze drying to prepare the edible chitosan-pectin gel balls capable of adsorbing heavy metals.
The chitosan-pectin gel beads prepared in this example were placed in a container containing Cu2+Oscillating for 7 hours in the water sample, and obtaining Cu in the original water sample2+The content of (2) is 101.9mg/L, and Cu in the water sample is adsorbed for 7 hours2+The content of (A) is 1.1mg/L, and the adsorption rate reaches 98.9%.
Example 2
Cd adsorption device2+The preparation of the edible chitosan-pectin gel beads comprises the following steps:
step 1, preparing chitosan-pectin hydrosol: dissolving 2g of chitosan and 1g of pectin in 100mL of food-grade hydrochloric acid solution with the acidity value of 1, and uniformly stirring at room temperature to prepare chitosan-pectin hydrosol;
step 2, preparing chitosan-pectin wet gel balls: slowly dripping the chitosan-pectin hydrosol prepared in the step 1 into 1mol/L edible caustic soda flakes solution drop by drop to obtain light yellow chitosan-pectin wet gel balls;
step 3, preparing chitosan-pectin gel beads: washing the chitosan-pectin wet gel balls prepared in the step 2 with distilled water to be neutral, and then placing the gel balls in a freeze dryer (FD-IC vacuum freeze dryer, Telstar company, Spain) (-50 ℃, 48h) for freeze drying to prepare the edible chitosan-pectin gel balls capable of adsorbing heavy metals.
The chitosan-pectin gel beads prepared in this example were placed in a container containing Cd2+Oscillating for 6 hours in the water sample, and adding Cd in the original water sample2+The content of the Cd in the water sample is 105.0mg/L, and the Cd in the water sample is adsorbed for 6 hours2+The content of (A) is 5.8mg/L, and the adsorption rate reaches 94.4%.
Example 3
Hg adsorption device2+The preparation of the edible chitosan-pectin gel beads comprises the following steps:
step 1, preparing chitosan-pectin hydrosol: dissolving 2g of chitosan and 1g of pectin in 100mL of food-grade hydrochloric acid solution with the acidity value of 1, and uniformly stirring at room temperature to prepare chitosan-pectin hydrosol;
step 2, preparing chitosan-pectin wet gel balls: slowly dripping the chitosan-pectin hydrosol prepared in the step 1 into 1-2 mol/L edible caustic soda flakes solution drop by drop to obtain light yellow chitosan-pectin wet gel balls;
step 3, preparing chitosan-pectin gel beads: washing the chitosan-pectin wet gel balls prepared in the step 2 with distilled water to be neutral, and then placing the gel balls in a freeze dryer (FD-IC vacuum freeze dryer, Telstar company, Spain) (-50 ℃, 48h) for freeze drying to prepare the edible chitosan-pectin gel balls capable of adsorbing heavy metals.
The chitosan-pectin gel beads prepared in this example were placed in a container containing Hg2+The water sample is oscillated for 8 hours, and Hg in the original water sample2+The content of the Hg in the water sample is 104.0mg/L, and the Hg in the water sample is adsorbed for 8 hours2+The content of (A) is 3.6mg/L, and the adsorption rate reaches 96.6%.
Example 4
Adsorb Pb2+Preparation of edible chitosan-pectin gel beads
Step 1, preparing chitosan-pectin hydrosol: dissolving 2g of chitosan and 1g of pectin in 100mL of food-grade hydrochloric acid solution with the acidity value of 1, and uniformly stirring at room temperature to prepare chitosan-pectin hydrosol;
step 2, preparing chitosan-pectin wet gel balls: slowly dripping the chitosan-pectin hydrosol prepared in the step 1 into 1mol/L edible caustic soda flakes solution drop by drop to obtain light yellow chitosan-pectin wet gel balls;
step 3, preparing chitosan-pectin gel beads: washing the chitosan-pectin wet gel balls prepared in the step 2 with distilled water to be neutral, and then placing the gel balls in a freeze dryer (FD-IC vacuum freeze dryer, Telstar company, Spain) (-50 ℃, 48h) for freeze drying to prepare the edible chitosan-pectin gel balls capable of adsorbing heavy metals.
The chitosan-pectin gel beads prepared in this example were placed in a container containing Pb2+Oscillating for 2 hours in the water sample, and obtaining Pb in the original water sample2+The content of the Pb in the water sample is 96.2mg/L, and the Pb in the water sample is adsorbed for 2 hours2+The content of (A) is 4.1mg/L, and the adsorption rate reaches 95.7%.
Claims (7)
1. A preparation method of edible chitosan-pectin gel beads for adsorbing heavy metals is characterized by comprising the following steps: the method comprises the following steps:
step 1, preparing chitosan-pectin hydrosol: dissolving chitosan and pectin in hydrochloric acid solution, and stirring to obtain chitosan-pectin hydrosol;
step 2, preparing chitosan-pectin wet gel balls: slowly dripping the chitosan-pectin hydrosol prepared in the step 1 into caustic soda flake solution drop by drop to prepare chitosan-pectin wet gel balls;
step 3, preparing chitosan-pectin gel beads: washing the chitosan-pectin wet gel balls prepared in the step 2 to be neutral by using distilled water, and then carrying out freeze drying to prepare the edible chitosan-pectin gel beads capable of adsorbing heavy metals.
2. The method for preparing the edible chitosan-pectin gel bead for adsorbing heavy metals according to claim 1, wherein:
in the step 1, the mass concentration of the chitosan is 0.01g/mL to 0.05g/mL, and the mass concentration of the pectin is 0.01g/mL to 0.05 g/mL.
3. The method for preparing the edible chitosan-pectin gel bead for adsorbing heavy metals according to claim 1, wherein:
the hydrochloric acid solution in the step 1 is a food grade hydrochloric acid solution, and the pH value of the hydrochloric acid solution is 1-2.
4. The method for preparing the edible chitosan-pectin gel bead for adsorbing heavy metals according to claim 1, wherein:
the caustic soda flake solution in the step 2 is a food-grade caustic soda flake solution, and the concentration of the caustic soda flake solution is 1 mol/L-2 mol/L.
5. The method for preparing the edible chitosan-pectin gel bead for adsorbing heavy metals according to claim 1, wherein:
in the step 3, the temperature of freeze drying is-80 ℃ to-50 ℃, and the time of freeze drying is 24h to 48 h.
6. Use of the edible chitosan-pectin gel beads for adsorbing heavy metals prepared according to the preparation method of claims 1 to 5, wherein: the method is used for adsorbing heavy metal ions in a water sample.
7. Use according to claim 6, characterized in that: the heavy metal ions include: cu2+、Cd2+、Hg2+And Pb2 +。
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| CN102380348A (en) * | 2011-09-21 | 2012-03-21 | 湖南大学 | Pectin modified magnetic nano-adsorbent and preparation method and application thereof |
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2021
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