CN111013547A - Composite heavy metal adsorbent and preparation method thereof - Google Patents
Composite heavy metal adsorbent and preparation method thereof Download PDFInfo
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- CN111013547A CN111013547A CN201911353921.5A CN201911353921A CN111013547A CN 111013547 A CN111013547 A CN 111013547A CN 201911353921 A CN201911353921 A CN 201911353921A CN 111013547 A CN111013547 A CN 111013547A
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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
- B01J20/10—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising silica or silicate
- B01J20/16—Alumino-silicates
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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
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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 composite heavy metal adsorbent and a preparation method thereof, wherein the composite heavy metal adsorbent comprises the following substances in parts by weight: 48-60 parts of attapulgite, 6-8 parts of PHEMA, 6-8 parts of ethylenediamine, 10-12 parts of chelating agent, 14-18 parts of chitosan, 80-120 parts of zeolite, 30-40 parts of acrylic resin and 18-24 parts of curing agent. According to the method, zeolite is subjected to corrosion treatment by an acetic acid solution, so that the pore density in the zeolite can be further increased, the specific surface area of the zeolite is increased, the zeolite is used as a carrier, after attapulgite, chitosan and EDA-PHEMA-chelating agents are complexed with each other, the zeolite is attached and fixed in pores of the zeolite through an ultraviolet curing agent and acrylic resin, an adsorbent is not easy to decompose after being cured, the use time is long, a stable adsorption system can be formed by compounding, and heavy metal ions in water can be effectively adsorbed.
Description
Technical Field
The invention belongs to the technical field of adsorbents, and particularly relates to a composite heavy metal adsorbent and a preparation method thereof.
Background
The heavy metal adsorbent is a treatment agent which is often adopted for treating heavy metal pollution of a water body. At present, the heavy metal adsorbent is not beneficial to simultaneously capturing various heavy metal ions in a water body due to single component, and has low adsorption efficiency on the heavy metal ions in the water body. And along with the increase of the existing time of the adsorbent in the sewage, the adsorbent is easy to decompose, and the adsorbent is unstable, so that the adsorption effect on heavy metals is influenced.
Disclosure of Invention
The invention aims to provide a composite heavy metal adsorbent and a preparation method thereof, and aims to solve the problems in the background technology.
In order to achieve the purpose, the invention provides the following technical scheme: a composite heavy metal adsorbent comprises the following substances in parts by weight:
48-60 parts of attapulgite, 6-8 parts of PHEMA, 6-8 parts of ethylenediamine, 10-12 parts of chelating agent, 14-18 parts of chitosan, 80-120 parts of zeolite, 30-40 parts of acrylic resin and 18-24 parts of curing agent.
Preferably, the chelating agent is one of xanthate derivatives, dithiocarbamate derivatives and Cibacron Blue F3 GA.
Preferably, the curing agent is an ultraviolet curing agent.
Preferably, the zeolite particles have a particle size of 2 to 4 mm.
Meanwhile, the invention also discloses a preparation method of the composite heavy metal adsorbent, which comprises the following operation steps:
s1: adding PHEMA into deionized water, mixing and stirring uniformly, adding equivalent amount of ethylenediamine, stirring in a water bath at 46-48 ℃ for 12-18 hours, derivatizing with ethylenediamine to obtain an EDA-PHEMA solution, adding a chelating agent, raising the temperature of the water bath to 80 ℃, continuing to stir for 4-6 hours to enable the chelating agent to be combined with the EDA-PHEMA, finally dropwise adding a 40% sodium hydroxide solution, and adjusting the concentration of the solution to be neutral to obtain the EDA-PHEMA-chelating agent solution for later use;
s2: putting the attapulgite, the chitosan and the cleaned zeolite into a mixer for uniform premixing, adding an EDA-PHEMA-chelating agent solution in S1 into the mixer, simultaneously adding deionized water, adjusting all substances to be emulsion, heating the mixer to 60-70 ℃, and continuously mixing for 4-8 hours to ensure that the attapulgite, the chitosan and the EDA-PHEMA-chelating agent are mutually complexed and attached to the pores of the zeolite;
s3: uniformly mixing acrylic resin and a curing agent under a dark condition, adding the acrylic resin and the curing agent into a mixer in S2, and continuously mixing for 3-5 hours under the dark condition;
s4: and after mixing is finished, filtering the mixed system by using a 200-mesh filter screen, collecting the filtered matter, scattering residual attapulgite on the filtered matter to form a coating structure to form a nuclear matter, uniformly mixing and stirring, simultaneously performing curing illumination by using an ultraviolet lamp, performing illumination treatment for 12-18 hours, after curing, soaking and cleaning by using clear water to remove redundant attapulgite on the surface, filtering again, and then placing in a 50-55 ℃ drying oven for drying to obtain the composite heavy metal adsorbent.
Preferably, the solute mass fractions of PHEMA and ethylenediamine in step S1 are both 15-20%.
Preferably, the attapulgite in the step S2 is attapulgite modified and activated by a silane coupling agent, and the zeolite is obtained by soaking in an acetic acid solution with PH of 5-6 for 2-3 hours and washing with clear water at 60 ℃.
The invention has the technical effects and advantages that:
according to the method, zeolite is subjected to corrosion treatment by an acetic acid solution, so that the pore density in the zeolite can be further increased, the specific surface area of the zeolite is increased, the zeolite is used as a carrier, after attapulgite, chitosan and EDA-PHEMA-chelating agents are complexed with each other, the zeolite is attached and fixed in pores of the zeolite through an ultraviolet curing agent and acrylic resin, an adsorbent is not easy to decompose after being cured, the use time is long, a stable adsorption system can be formed by compounding, and heavy metal ions in water can be effectively adsorbed.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the embodiments of the present invention, and it is obvious 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 derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1
A composite heavy metal adsorbent comprises the following substances in parts by weight:
48 parts of attapulgite, 6 parts of PHEMA, 6 parts of ethylenediamine, 10 parts of chelating agent, 14 parts of chitosan, 80 parts of zeolite, 30 parts of acrylic resin and 18 parts of curing agent.
The chelating agent is xanthate derivatives.
The curing agent is an ultraviolet curing agent.
The particle size of the zeolite particles is 2 mm.
Meanwhile, the invention also discloses a preparation method of the composite heavy metal adsorbent, which comprises the following operation steps:
s1: adding PHEMA into deionized water, mixing and stirring uniformly, adding equivalent amount of ethylenediamine, stirring for 12 hours in a water bath at 46 ℃, derivatizing with ethylenediamine to obtain an EDA-PHEMA solution, adding a chelating agent, raising the temperature of the water bath to 80 ℃, continuing stirring for 4 hours to enable the chelating agent to be combined with the EDA-PHEMA, finally dropwise adding a 40% sodium hydroxide solution, and adjusting the concentration of the solution to be neutral to obtain the EDA-PHEMA-chelating agent solution for later use;
s2: putting attapulgite, chitosan and cleaned zeolite into a mixer for uniform premixing, adding an EDA-PHEMA-chelating agent solution in S1 into the mixer, simultaneously adding deionized water, adjusting all substances to be emulsion, heating the mixer to 60 ℃, and continuously mixing for 4 hours to ensure that the attapulgite, the chitosan and the EDA-PHEMA-chelating agent are mutually complexed and attached to the pores of the zeolite;
s3: uniformly mixing acrylic resin and a curing agent under a dark condition, adding the acrylic resin and the curing agent into a mixer in S2, and continuously mixing for 3 hours under the dark condition;
s4: and after mixing is finished, filtering a mixing system by using a 200-mesh filter screen, collecting a filtered substance, scattering residual attapulgite on the filtered substance to form a coating structure to form a nuclear substance, uniformly mixing and stirring, simultaneously performing curing illumination by using an ultraviolet lamp, performing illumination treatment for 12 hours, after curing is finished, soaking and cleaning by using clear water to remove the redundant attapulgite on the surface, filtering again, and drying in a 50-55 ℃ oven to obtain the composite heavy metal adsorbent.
In step S1, the solute mass fractions of PHEMA and ethylenediamine are both 15%.
In the step S2, the attapulgite is modified and activated by a silane coupling agent, and the zeolite is obtained by soaking in an acetic acid solution with a PH of 5 for 2 hours and washing with clear water at 60 ℃.
Example 2
A composite heavy metal adsorbent comprises the following substances in parts by weight:
54 parts of attapulgite, 7 parts of PHEMA, 7 parts of ethylenediamine, 11 parts of chelating agent, 16 parts of chitosan, 100 parts of zeolite, 35 parts of acrylic resin and 21 parts of curing agent.
The chelating agent is dithiocarbamate derivatives.
The curing agent is an ultraviolet curing agent.
The particle size of the zeolite particles is 3 mm.
Meanwhile, the invention also discloses a preparation method of the composite heavy metal adsorbent, which comprises the following operation steps:
s1: adding PHEMA into deionized water, mixing and stirring uniformly, adding equivalent amount of ethylenediamine, stirring for 15 hours in a water bath at 47 ℃, derivatizing with ethylenediamine to obtain an EDA-PHEMA solution, adding a chelating agent, raising the temperature of the water bath to 80 ℃, continuing stirring for 5 hours to enable the chelating agent to be combined with the EDA-PHEMA, finally dropwise adding a 40% sodium hydroxide solution, and adjusting the concentration of the solution to be neutral to obtain the EDA-PHEMA-chelating agent solution for later use;
s2: putting attapulgite, chitosan and cleaned zeolite into a mixer for uniform premixing, adding an EDA-PHEMA-chelating agent solution in S1 into the mixer, simultaneously adding deionized water, adjusting all substances to be emulsion, heating the mixer to 65 ℃, and continuously mixing for 6 hours to ensure that the attapulgite, the chitosan and the EDA-PHEMA-chelating agent are mutually complexed and attached to the pores of the zeolite;
s3: uniformly mixing acrylic resin and a curing agent under a dark condition, adding the acrylic resin and the curing agent into a mixer in S2, and continuously mixing for 4 hours under the dark condition;
s4: after mixing, filtering a mixing system by using a 200-mesh filter screen, collecting a filtered substance, scattering residual attapulgite on the filtered substance to form a coating structure, forming a nuclear substance, uniformly mixing and stirring, simultaneously performing curing illumination by using an ultraviolet lamp, performing illumination treatment for 15 hours, soaking and cleaning the residual attapulgite in clear water to remove the redundant attapulgite on the surface after curing, filtering again, and drying in a 53-DEG C oven to obtain the composite heavy metal adsorbent.
In step S1, both the solute mass fractions of PHEMA and ethylenediamine are 18%.
In the step S2, the attapulgite is modified and activated by a silane coupling agent, and the zeolite is soaked in an acetic acid solution with a PH of 5.5 for 2.5 hours and washed with clear water at 60 ℃.
Example 3
A composite heavy metal adsorbent comprises the following substances in parts by weight:
60 parts of attapulgite, 8 parts of PHEMA, 8 parts of ethylenediamine, 12 parts of chelating agent, 18 parts of chitosan, 120 parts of zeolite, 40 parts of acrylic resin and 24 parts of curing agent.
The chelating agent is Cibacron Blue F3 GA.
The curing agent is an ultraviolet curing agent.
The particle size of the zeolite particles is 4 mm.
Meanwhile, the invention also discloses a preparation method of the composite heavy metal adsorbent, which comprises the following operation steps:
s1: adding PHEMA into deionized water, mixing and stirring uniformly, adding equivalent amount of ethylenediamine, stirring for 18 hours in a water bath at 48 ℃, derivatizing with ethylenediamine to obtain an EDA-PHEMA solution, adding a chelating agent, raising the temperature of the water bath to 80 ℃, continuing stirring for 6 hours to enable the chelating agent to be combined with the EDA-PHEMA, finally dropwise adding a 40% sodium hydroxide solution, and adjusting the concentration of the solution to be neutral to obtain the EDA-PHEMA-chelating agent solution for later use;
s2: putting attapulgite, chitosan and cleaned zeolite into a mixer for uniform premixing, adding an EDA-PHEMA-chelating agent solution in S1 into the mixer, simultaneously adding deionized water, adjusting all substances to be emulsion, heating the mixer to 70 ℃, and continuously mixing for 8 hours to ensure that the attapulgite, the chitosan and the EDA-PHEMA-chelating agent are mutually complexed and attached to the pores of the zeolite;
s3: uniformly mixing acrylic resin and a curing agent under a dark condition, adding the acrylic resin and the curing agent into a mixer in S2, and continuously mixing for 5 hours under the dark condition;
s4: after mixing, filtering a mixing system by using a 200-mesh filter screen, collecting filtered substances, scattering residual attapulgite on the filtered substances to form a coating structure, forming a nuclear substance, uniformly mixing and stirring, simultaneously performing curing illumination by using an ultraviolet lamp, performing illumination treatment for 18 hours, soaking and cleaning the residual attapulgite in clear water to remove the redundant attapulgite on the surface after curing, filtering again, and drying in a 55-DEG C oven to obtain the composite heavy metal adsorbent.
In step S1, both the solute mass fractions of PHEMA and ethylenediamine are 20%.
In the step S2, the attapulgite is modified and activated by a silane coupling agent, and the zeolite is obtained by soaking in an acetic acid solution with a PH of 6 for 3 hours and washing with clear water at 60 ℃.
According to the method, zeolite is subjected to corrosion treatment by an acetic acid solution, so that the pore density in the zeolite can be further increased, the specific surface area of the zeolite is increased, the zeolite is used as a carrier, after attapulgite, chitosan and EDA-PHEMA-chelating agents are complexed with each other, the zeolite is attached and fixed in pores of the zeolite through an ultraviolet curing agent and acrylic resin, an adsorbent is not easy to decompose after being cured, the use time is long, a stable adsorption system can be formed by compounding, and heavy metal ions in water can be effectively adsorbed.
Finally, it should be noted that: although the present invention has been described in detail with reference to the foregoing embodiments, it will be apparent to those skilled in the art that modifications may be made to the embodiments or portions thereof without departing from the spirit and scope of the invention.
Claims (7)
1. A compound heavy metal adsorbent is characterized in that: the material comprises the following substances in parts by weight:
48-60 parts of attapulgite, 6-8 parts of PHEMA, 6-8 parts of ethylenediamine, 10-12 parts of chelating agent, 14-18 parts of chitosan, 80-120 parts of zeolite, 30-40 parts of acrylic resin and 18-24 parts of curing agent.
2. The composite heavy metal adsorbent of claim 1, wherein: the chelating agent is one of xanthate derivatives, dithiocarbamate derivatives or Cibacron Blue F3 GA.
3. The composite heavy metal adsorbent of claim 1, wherein: the curing agent is an ultraviolet curing agent.
4. The composite heavy metal adsorbent of claim 1, wherein: the particle size of the zeolite particles is 2-4 mm.
5. A method for preparing the composite heavy metal adsorbent according to any one of claims 1 to 4, wherein: the method comprises the following operation steps:
s1: adding PHEMA into deionized water, mixing and stirring uniformly, adding equivalent amount of ethylenediamine, stirring in a water bath at 46-48 ℃ for 12-18 hours, derivatizing with ethylenediamine to obtain an EDA-PHEMA solution, adding a chelating agent, raising the temperature of the water bath to 80 ℃, continuing to stir for 4-6 hours to enable the chelating agent to be combined with the EDA-PHEMA, finally dropwise adding a 40% sodium hydroxide solution, and adjusting the concentration of the solution to be neutral to obtain the EDA-PHEMA-chelating agent solution for later use;
s2: putting the attapulgite, the chitosan and the cleaned zeolite into a mixer for uniform premixing, adding an EDA-PHEMA-chelating agent solution in S1 into the mixer, simultaneously adding deionized water, adjusting all substances to be emulsion, heating the mixer to 60-70 ℃, and continuously mixing for 4-8 hours to ensure that the attapulgite, the chitosan and the EDA-PHEMA-chelating agent are mutually complexed and attached to the pores of the zeolite;
s3: uniformly mixing acrylic resin and a curing agent under a dark condition, adding the acrylic resin and the curing agent into a mixer in S2, and continuously mixing for 3-5 hours under the dark condition;
s4: and after mixing is finished, filtering the mixed system by using a 200-mesh filter screen, collecting the filtered matter, scattering residual attapulgite on the filtered matter to form a coating structure to form a nuclear matter, uniformly mixing and stirring, simultaneously performing curing illumination by using an ultraviolet lamp, performing illumination treatment for 12-18 hours, after curing, soaking and cleaning by using clear water to remove redundant attapulgite on the surface, filtering again, and then placing in a 50-55 ℃ drying oven for drying to obtain the composite heavy metal adsorbent.
6. The preparation method of the composite heavy metal adsorbent according to claim 5, wherein the preparation method comprises the following steps: in step S1, the solute mass fractions of PHEMA and ethylenediamine are both 15-20%.
7. The preparation method of the composite heavy metal adsorbent according to claim 5, wherein the preparation method comprises the following steps: in the step S2, the attapulgite is modified and activated by a silane coupling agent, the zeolite is soaked in an acetic acid solution with the pH of 5-6 for 2-3 hours, and the zeolite is obtained by cleaning with clear water at 60 ℃.
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Cited By (2)
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| CN111744463A (en) * | 2020-06-29 | 2020-10-09 | 重庆工程职业技术学院 | Heavy metal composite passivator for sludge treatment |
| CN112552811A (en) * | 2020-12-12 | 2021-03-26 | 北京宇阳泽丽防水材料有限责任公司 | Environment-friendly one-component polyurethane waterproof coating and preparation method thereof |
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| CN112552811A (en) * | 2020-12-12 | 2021-03-26 | 北京宇阳泽丽防水材料有限责任公司 | Environment-friendly one-component polyurethane waterproof coating and preparation method thereof |
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