CN112958053A - Preparation method and application of PG/PAA composite aerogel - Google Patents

Preparation method and application of PG/PAA composite aerogel Download PDF

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CN112958053A
CN112958053A CN202110331157.2A CN202110331157A CN112958053A CN 112958053 A CN112958053 A CN 112958053A CN 202110331157 A CN202110331157 A CN 202110331157A CN 112958053 A CN112958053 A CN 112958053A
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composite aerogel
paa composite
gel
preparation
deionized water
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CN112958053B (en
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陈志军
潘志恒
杨清香
赵俊红
谢云鹏
王青青
王芳草
王聪
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Zhengzhou University of Light Industry
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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
    • B01J20/26—Synthetic macromolecular compounds
    • B01J20/261—Synthetic macromolecular compounds obtained by reactions only involving carbon to carbon unsaturated bonds
    • 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
    • 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
    • B01J20/28047—Gels
    • 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
    • B01J20/30—Processes for preparing, regenerating, or reactivating
    • B01J20/3071—Washing or leaching
    • 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
    • B01J20/30—Processes for preparing, regenerating, or reactivating
    • B01J20/3085—Chemical treatments not covered by groups B01J20/3007 - B01J20/3078
    • 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
    • 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
    • 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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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Analytical Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Hydrology & Water Resources (AREA)
  • Engineering & Computer Science (AREA)
  • Environmental & Geological Engineering (AREA)
  • Water Supply & Treatment (AREA)
  • Dispersion Chemistry (AREA)
  • Solid-Sorbent Or Filter-Aiding Compositions (AREA)

Abstract

The invention provides a preparation method and application of PG/PAA composite aerogel, which comprises the following steps: (1) placing peach gum in a beaker, adding acrylic acid, potassium persulfate and deionized water for swelling; (2) pouring the swollen product into a reaction kettle for hydrothermal reaction to form gel, taking out the gel, cooling the gel to room temperature, washing the gel with water, and adding deionized water for swelling again; (3) and (3) freezing and crystallizing the material swelled in the step (2), and then freezing and drying to obtain the PG/PAA composite aerogel. The invention utilizes the structural characteristics of a large amount of hydroxyl and carboxyl in peach gum and the advantages of low toxicity, easy obtaining and low cost of biomass base materials, takes acrylic acid as a cross-linking agent, and adopts a hydrothermal method to prepare the water-based PG/PAA composite aerogel. The solvent used in the preparation process is deionized water, so that the cost is reduced, and the environment is not polluted.

Description

Preparation method and application of PG/PAA composite aerogel
Technical Field
The invention relates to the field of sewage treatment, and in particular relates to a preparation method and application of PG/PAA composite aerogel.
Background
Industrialization and increasing consumption lead to an increase in the degree of contamination of industrial sources, posing a potential threat to ecosystem. Among them, water pollution caused by heavy metal ions is one of the hot spots of great concern in most countries. Cadmium (Cd), chromium (Cr), copper (Cu), lead (Pb), nickel (Ni), cobalt (Co), etc. are the most common heavy metal pollutants in industrial pollution, and their main sources include mineral processing, leather, tanneries, metal plating, steel production, pesticides, etc. Heavy metal ions enter the food chain easily through different routes and accumulate gradually in the life cycle, producing progressive toxic effects, possibly leading to bone degeneration, damage to the liver and lungs and even the blood, etc. The removal of heavy metals is therefore of great interest and it is necessary to take certain measures to treat the waste water discharged into the environment. The existing methods for removing heavy metal ions include chemical precipitation, biological treatment, ion exchange, adsorption, filtration and the like. Among various methods for treating wastewater, the adsorption method has the characteristics of rapidness, high selectivity and high efficiency, has wide application prospect in the aspect of removing heavy metals in wastewater, and arouses the interest of numerous researchers.
Peach gum Polysaccharide (PG), a natural acidic heteropolysaccharide, is produced by mechanical or physiological damage to the trunks and fruits of Peach trees, and PG has a highly branched macromolecular structure generally consisting of arabinose, galactose, uronic acid, xylose, and mannose. PG has shown wide application prospects in the food industry such as medicines, adsorbents, sensors, fluorescent materials and the like so far. Since PG contains a large amount of hydroxyl and carboxyl groups, PG-based aerogels are expected to exhibit better metal ion chelating or adsorbing properties. In addition, peach gum raw materials are abundant in many parts of the world, and therefore peach gum is low in cost and readily available.
Disclosure of Invention
The invention provides a preparation method and application of PG/PAA composite aerogel.
The technical scheme for realizing the invention is as follows:
a preparation method of PG/PAA composite aerogel comprises the following steps:
(1) placing peach gum in a beaker, adding acrylic acid, potassium persulfate and deionized water for swelling;
(2) pouring the swollen product into a reaction kettle for hydrothermal reaction to form gel, taking out the gel, cooling the gel to room temperature, washing the gel with water, and adding deionized water for swelling again;
(3) and (3) freezing and crystallizing the material swelled in the step (2), and then freezing and drying to obtain the PG/PAA composite aerogel.
In the step (1), the mass ratio of the peach gum to the acrylic acid to the potassium persulfate to the deionized water is 1:1:0.1: 5.
The hydrothermal reaction temperature in the step (2) is 80-100 ℃, the time is 8-12h, and the re-swelling time is 24-36 h.
The temperature of the frozen crystals in the step (3) is-18 ℃ to-20 ℃, the time is 12h to 24h, and the temperature of the frozen crystals is-45 ℃ to-55 ℃, and the time is 1h to 36 h.
The prepared PG/PAA composite aerogel is applied to adsorption of heavy metal ions.
The concentration of the heavy metal ion solution is 300mg/L, and 20mg of PG/PAA composite aerogel is added into every 40mL of solution.
The pH value of the heavy metal ion solution is 2.0-7.0.
The invention has the beneficial effects that: the invention utilizes the structural characteristics of a large amount of hydroxyl and carboxyl in peach gum and the advantages of low toxicity, easy obtaining and low cost of biomass base materials, takes acrylic acid as a cross-linking agent, and adopts a hydrothermal method to prepare the water-based PG/PAA composite aerogel. The solvent used in the preparation process is deionized water, so that the cost is reduced, and the environment is not polluted. The peach gum is used as the biological base material, and the prepared PG/PAA composite aerogel has good adsorption performance on heavy metal ions due to the fact that the porous structure of the composite aerogel provides a large number of adsorption sites for adsorbing the heavy metal ions.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, it is obvious that the drawings in the following description are only some embodiments of the present invention, and for those skilled in the art, other drawings can be obtained according to the drawings without creative efforts.
FIG. 1 is an SEM image of a PG/PAA composite aerogel of the present invention.
FIG. 2 is an XRD pattern of PG, PG/PAA composite aerogel.
FIG. 3 is a FT-IR diagram of PG, PG/PAA composite aerogel.
Detailed Description
The technical solutions of the present invention will be described clearly and completely with reference to the following embodiments of the present invention, and it should be understood that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be obtained by a person skilled in the art without inventive effort based on the embodiments of the present invention, are within the scope of the present invention.
Examples
The preparation method of the aerogel comprises the following steps:
(1) preparation of gel: putting 1.0g of peach gum into a beaker, adding 1.0g of Acrylic Acid (AA), 0.1g of potassium persulfate and 5.0 mL of deionized water, swelling for more than 24h, pouring the reactant into a reaction kettle with a polytetrafluoroethylene lining after swelling is finished, adding 5mL of deionized water, and carrying out hydrothermal reaction on the mixed solution at 80-100 ℃ for 8 hours to form gel.
(3) Preparing aerogel: and taking out the gel, cooling the gel to room temperature in the air, washing the gel with water to remove unreacted AA, washing the gel with deionized water for 2 to 3 times, and adding a proper amount of water into the gel to swell for more than 30 hours. Transferring the obtained product to a refrigerator freezing layer for freezing crystallization at-18 to-20 ℃ for 24 hours after swelling is finished, removing the product from the freezing layer, and performing freeze drying in a freeze dryer at-45 to-55 ℃ for more than 1 to 36 hours to obtain the PG/PAA composite aerogel.
The experimental results are as follows:
FIG. 1 is an SEM image of PG/PAA composite aerogel, wherein (a) X80000, (b) X50000, and (c) X30000. Fig. 1 shows that the prepared composite aerogel has a rough surface and a uniform porous structure inside the composite sample. The functional group (-OH) on the peach gum is supposed to have a crosslinking effect with-COOH on polyacrylic acid, the porous structure is formed by peach gum and polyacrylic acid polymer, and the porous structure of PG/PAA increases the specific surface area of the composite aerogel, provides more adsorption sites and improves the adsorptivity of the composite aerogel to heavy metal ions to a certain extent.
Fig. 2 is an XRD pattern of PG/PAA composite aerogel, the PG/PAA composite aerogel belongs to a polymer material, and there is no crystal diffraction peak on the XRD pattern, but there is an amorphous dispersion peak around 2 θ =20 °, which meets the amorphous characteristic. FIG. 3 is the FT-IR spectrum of PG/PAA at a wave number of 3466 cm-1And 1035 cm-1The absorption peaks of (A) are respectively related to O-H vibration and C-O vibration, and the wave number of the composite aerogel is 1729 cm-1An absorption peak appeared, and it was judged as a C = O stretching vibration peak. By analyzing the infrared spectrogram and the XRD pattern, the PG/PAA composite aerogel can be presumed to be successfully prepared.
The adsorption experiment result shows that the PG/PAA composite aerogel has heavy metal ions (Pb)2+、Cd2+、Ni2+、Cu2+、Co2+) Has good adsorption performance on Pb under the conditions that the pH is about 5, the adsorption time is 8 hours, 20mg of adsorbent and the concentration of a heavy metal ion solution is 300mg/L2+The adsorption capacity reaches 246.86mg/g, and the adsorption capacity is specific to Cd2+The adsorption capacity reaches 121.62mg/g, for Ni2+The adsorption capacity reaches 151.33mg/g, for Cu2+The adsorption capacity reaches 136.38mg/g, and the adsorption capacity to Co2+The adsorption capacity reaches 158.19 mg/g.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents, improvements and the like that fall within the spirit and principle of the present invention are intended to be included therein.

Claims (7)

1. A preparation method of PG/PAA composite aerogel is characterized by comprising the following steps:
(1) placing peach gum in a beaker, adding acrylic acid, potassium persulfate and deionized water for swelling;
(2) pouring the swollen product into a reaction kettle for hydrothermal reaction to form gel, taking out the gel, cooling the gel to room temperature, washing the gel with water, and adding deionized water for swelling again;
(3) and (3) freezing and crystallizing the material swelled in the step (2), and then freezing and drying to obtain the PG/PAA composite aerogel.
2. The preparation method of PG/PAA composite aerogel according to claim 1, characterized in that: in the step (1), the mass ratio of the peach gum to the acrylic acid to the potassium persulfate to the deionized water is 1:1:0.1: 5.
3. The preparation method of PG/PAA composite aerogel according to claim 1, characterized in that: the hydrothermal reaction temperature in the step (2) is 80-100 ℃, the time is 8-12h, and the re-swelling time is 24-36 h.
4. The preparation method of PG/PAA composite aerogel according to claim 1, characterized in that: the temperature of the frozen crystals in the step (3) is-18 ℃ to-20 ℃, the time is 12h to 24h, and the temperature of the frozen crystals is-45 ℃ to-55 ℃, and the time is 1h to 36 h.
5. Use of the PG/PAA composite aerogel prepared by the preparation method of any one of claims 1 to 4 in adsorption of heavy metal ions.
6. Use according to claim 5, characterized in that: the concentration of the heavy metal ion solution is 300mg/L, and 20mg of PG/PAA composite aerogel is added into every 40mL of solution.
7. Use according to claim 6, characterized in that: the pH value of the heavy metal ion solution is 2.0-7.0.
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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114471095A (en) * 2022-02-11 2022-05-13 苏州北美国际高级中学 Organic aerogel desiccant and preparation method thereof
CN114477134A (en) * 2022-02-11 2022-05-13 苏州北美国际高级中学 Carbon aerogel material and preparation method thereof

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103044720A (en) * 2013-01-19 2013-04-17 桂林理工大学 Preparation method of magnetic peach gum
CN104945639A (en) * 2015-06-17 2015-09-30 华南理工大学 Sulfur-containing modified chitosan containing aerogel as well as preparation method and application thereof
CN106008840A (en) * 2016-06-30 2016-10-12 广州振清环保技术有限公司 Chitosan crosslinked modified resin as well as preparation method and application thereof
CN109574187A (en) * 2018-12-26 2019-04-05 大连理工大学 A kind of multi-stage nano gel photo-reduction co-precipitation recycling heavy metal ion method

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103044720A (en) * 2013-01-19 2013-04-17 桂林理工大学 Preparation method of magnetic peach gum
CN104945639A (en) * 2015-06-17 2015-09-30 华南理工大学 Sulfur-containing modified chitosan containing aerogel as well as preparation method and application thereof
CN106008840A (en) * 2016-06-30 2016-10-12 广州振清环保技术有限公司 Chitosan crosslinked modified resin as well as preparation method and application thereof
CN109574187A (en) * 2018-12-26 2019-04-05 大连理工大学 A kind of multi-stage nano gel photo-reduction co-precipitation recycling heavy metal ion method

Non-Patent Citations (2)

* Cited by examiner, † Cited by third party
Title
BO HUANG，ET AL: ""Versatile magnetic gel from peach gum polysaccharide for efficient adsorption of Pb2+ and Cd2+ ions and catalysis"" *
JISUAN TAN，ET AL: ""Facile Functionalization of Natural Peach Gum Polysaccharide with Multiple Amine Groups for Highly Efficient Removal of Toxic Hexavalent Chromium (Cr(VI)) Ions from Water"" *

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114471095A (en) * 2022-02-11 2022-05-13 苏州北美国际高级中学 Organic aerogel desiccant and preparation method thereof
CN114477134A (en) * 2022-02-11 2022-05-13 苏州北美国际高级中学 Carbon aerogel material and preparation method thereof
CN114471095B (en) * 2022-02-11 2024-02-09 苏州北美国际高级中学 Organic aerogel drying agent and preparation method thereof
CN114477134B (en) * 2022-02-11 2024-06-07 苏州北美国际高级中学 Carbon aerogel material and preparation method thereof

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