CN110665460A - Irradiation modified attapulgite/activated carbon composite carbon rod and preparation method thereof - Google Patents
Irradiation modified attapulgite/activated carbon composite carbon rod and preparation method thereof Download PDFInfo
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- CN110665460A CN110665460A CN201910958108.4A CN201910958108A CN110665460A CN 110665460 A CN110665460 A CN 110665460A CN 201910958108 A CN201910958108 A CN 201910958108A CN 110665460 A CN110665460 A CN 110665460A
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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
- B01J20/20—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising free carbon; comprising carbon obtained by carbonising processes
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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
- C02F1/281—Treatment of water, waste water, or sewage by sorption using inorganic 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
- C02F2101/12—Halogens or halogen-containing compounds
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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
- C02F2101/30—Organic compounds
- C02F2101/40—Organic compounds containing sulfur
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Abstract
The invention discloses a preparation method of an irradiation modified attapulgite/activated carbon composite carbon rod, which comprises the following steps: (1) dissolving attapulgite in water, carrying out acidification treatment, drying, grinding, and carrying out irradiation modification treatment; (2) mixing the irradiation modified attapulgite with activated carbon, dissolving in water, adding acetic acid, and roasting in a muffle furnace; (3) putting the composite material obtained in the step (2), a zinc oxide antibacterial agent, a binder and phosphate into a mixer, uniformly mixing, die-casting and molding, calcining at high temperature, and cooling to obtain an irradiation modified attapulgite composite carbon rod; the invention greatly increases the pore structure of the attapulgite after the acid treatment and the irradiation treatment, and the composite carbon rod prepared by compounding the attapulgite with the active carbon has high-efficiency adsorption performance and low preparation cost.
Description
Technical Field
The invention belongs to the technical field of active carbon processing, and particularly relates to an irradiation modified attapulgite/active carbon composite carbon rod for a water purification filter element and a preparation method thereof.
Background
With the acceleration of the urbanization process, the increase of urban population and the enhancement of environmental awareness, the discharge amount of urban industrial wastewater and domestic sewage is increasing day by day, the urban sewage treatment rate is also improved year by year, the sewage treatment can not be separated from the adsorbent, and the activated carbon is a porous adsorption material, has rich pore structure, higher specific surface area and strong adsorption capacity, is a very ideal environment-friendly adsorbent, and the activated carbon has the advantages of developed pores, good adsorption performance, high strength, easy regeneration, economy, durability and the like, and is widely applied to sewage treatment, for example, patent CN105536719A discloses a modified activated carbon adsorbent, which is composed of the following raw materials in parts by weight: 80-90 parts of coconut shell activated carbon, 80-85 parts of wood activated carbon, 60-70 parts of coal activated carbon, 20-25 parts of wheat straw, 10-15 parts of peanut shell, 30-40 parts of attapulgite, 5-10 parts of kaolin, 8-10 parts of vermiculite, 1-3 parts of methyl cellulose, 0.5-1 part of sodium dodecyl benzene sulfonate and 2-5 parts of an activating agent, wherein the activating agent is one or more of sodium hydroxide, potassium hydroxide and calcium oxide. The invention has large specific surface area, large adsorption capacity, high treatment degree, stable effect and no secondary pollution; however, in the technical scheme, the adopted activated carbon has more types, various auxiliary substances are required to be added to complete the modification of the modified activated carbon, the cost of the activated carbon is higher, and the manufacturing cost of the household water purifier industry is increased undoubtedly.
Disclosure of Invention
In order to solve the technical problems, the invention provides an irradiation modified attapulgite/activated carbon composite carbon rod and a preparation method thereof.
The technical scheme provided by the invention is as follows:
a preparation method of an irradiation modified attapulgite composite carbon rod comprises the following steps:
(1) dissolving attapulgite in water, carrying out acidification treatment, drying, grinding, placing on a high-energy electron beam irradiation conveyor belt, carrying out irradiation treatment, and grinding to obtain irradiation modified attapulgite;
(2) mixing the irradiation modified attapulgite with the activated carbon, dissolving in water, stirring uniformly, adding acetic acid, and roasting in a muffle furnace to obtain the irradiation modified attapulgite/activated carbon composite material;
(3) and (3) placing the irradiation modified attapulgite/activated carbon composite material obtained in the step (2), the zinc oxide antibacterial agent, the binder and the phosphate into a mixer to be uniformly mixed, die-casting and molding, calcining at high temperature, and cooling to obtain the irradiation modified attapulgite composite carbon rod.
Preferably, in the step (1), the reagent used for the acidification treatment is 1 ~ 2mol/L hydrochloric acid solution.
Preferably, in the step (1), the drying temperature is 60 ~ 80 ℃, and the drying time is 8 ~ 10 h.
Preferably, in the step (1), the irradiation energy of the high-energy electron beam is 10 ~ 20MeV, and the irradiation dose is 30 ~ 50 KGy.
Preferably, in the step (2), the stirring time is 5 ~ 6h, the roasting temperature is 400 ~ 500 ℃, and the time is 30 ~ 50 min.
Preferably, in the step (3), the mixing speed is 20 ~ 30r/min and the mixing time is 20 ~ 30 min.
Preferably, in the step (3), the calcining temperature is 550 ~ 650 ℃ and the calcining time is 1 ~ 2 h.
Preferably, in the step (2), the mass ratio of the irradiation modified attapulgite to the activated carbon is 10 (1 ~ 3).
Preferably, in the step (3), the mass ratio of the zinc oxide antibacterial agent to the irradiation modified attapulgite/activated carbon composite material is (4 ~ 5): 1.
An irradiation modified attapulgite composite carbon rod is prepared by the preparation method of the irradiation modified attapulgite composite carbon rod.
Compared with the prior art, the invention has the following technical advantages:
(1) the attapulgite modified adsorbent has the advantages that the attapulgite modified adsorbent is subjected to irradiation modification after being treated by the acid, has low cost and wide sources, has richer pore channel structures, improves the adsorption efficiency after being compounded with the activated carbon, can effectively prevent pore channel blockage of the activated carbon, and reduces the addition amount of the activated carbon in the composite material, so that the production cost is reduced, and the attapulgite modified adsorbent is beneficial to large-scale production and application;
(2) the invention utilizes high-energy electron beam irradiation to modify the attapulgite, and the process has no secondary pollution and simple and convenient operation;
(3) the invention utilizes the attapulgite to enhance the adsorption capacity of the activated carbon, has simple preparation process, low cost (200 ~ 1000 yuan/ton), high recycling rate, can be applied to the preposed filter element of the household water purifier, and has wide market application prospect.
Drawings
FIG. 1 is a scanning electron micrograph of untreated attapulgite
FIG. 2 is a scanning electron micrograph of an acid-treated attapulgite
FIG. 3 is a scanning electron microscope image of attapulgite clay after irradiation modification
FIG. 4 is a scanning electron micrograph of attapulgite modified by acid treatment and irradiation in example 1 of the present invention
FIG. 5 is a chart showing the results of the methyl blue adsorption test of the irradiation modified attapulgite/activated carbon composite material prepared in example 1 of the present invention
FIG. 6 is a graph showing the results of chlorine adsorption tests on the irradiation modified attapulgite/activated carbon composite material prepared in example 1 of the present invention.
Detailed Description
The invention will now be further described with reference to specific embodiments and drawings.
Example 1
A preparation method of an irradiation modified attapulgite composite carbon rod comprises the following steps:
(1) weighing 20 g of attapulgite, dissolving in 50 mL of deionized water, adding 1 mol/L hydrochloric acid for acidification pretreatment, transferring to a culture dish with the diameter of 10 cm, and drying at 60 ℃ for 10 h; grinding the dried sample, placing the ground sample on a high-energy electron beam irradiation conveyor belt, and performing irradiation treatment, wherein the high-energy electron beam irradiation energy is 10MeV, and the irradiation dose is 30 KGy, and grinding the sample after irradiation to obtain irradiation modified attapulgite;
(2) controlling the mass ratio of the irradiation modified attapulgite to the activated carbon to be 10:3, adding 50 mL deionized water, uniformly mixing, stirring for 6h, adding 2g acetic acid, placing in a muffle furnace, roasting at 450 ℃, and roasting for 40 min to obtain the irradiation modified attapulgite/activated carbon composite material;
(3) and (3) mixing the irradiation modified attapulgite/activated carbon composite material obtained in the step (2) with a zinc oxide antibacterial agent according to the mass ratio of 1:5, adding a binder and a phosphate, mixing for 30min at the speed of 20 r/min by using a mixer, die-casting and molding, calcining for 1h at the high temperature of 600 ℃, and cooling to obtain the irradiation modified attapulgite composite carbon rod.
Example 2
A preparation method of an irradiation modified attapulgite composite carbon rod comprises the following steps:
(1) weighing 20 g of attapulgite, dissolving in 50 mL of deionized water, adding 1.5mol/L hydrochloric acid for acidification pretreatment, transferring to a culture dish with the diameter of 10 cm, and drying for 9 h at 70 ℃; grinding the dried sample, placing the ground sample on a high-energy electron beam irradiation conveyor belt, performing irradiation treatment, wherein the high-energy electron beam irradiation energy is 15MeV, and the irradiation dose is 40 KGy, and grinding the sample after irradiation to obtain irradiation modified attapulgite;
(2) controlling the mass ratio of the irradiation modified attapulgite to the activated carbon to be 10:1, adding 50 mL of deionized water, uniformly mixing, stirring for 6h, adding 2g of acetic acid, placing in a muffle furnace, roasting at 400 ℃, and roasting for 50min to obtain the irradiation modified attapulgite/activated carbon composite material;
(3) and (3) mixing the irradiation modified attapulgite/activated carbon composite material obtained in the step (2) with a zinc oxide antibacterial agent according to a mass ratio of 1:4, adding a binder and a phosphate, mixing for 25 min at a speed of 25 r/min by using a mixer, die-casting and molding, calcining for 2h at a high temperature of 550 ℃, and cooling to obtain the irradiation modified attapulgite composite carbon rod.
Example 3
(1) Weighing 20 g of attapulgite, dissolving in 50 mL of deionized water, adding 2mol/L hydrochloric acid for acidification pretreatment, transferring to a culture dish with the diameter of 10 cm, and drying for 8 h at 80 ℃; grinding the dried sample, placing the ground sample on a high-energy electron beam irradiation conveyor belt, and performing irradiation treatment, wherein the high-energy electron beam irradiation energy is 20MeV, and the irradiation dose is 50KGy, and grinding the sample after irradiation to obtain irradiation modified attapulgite;
(2) controlling the mass ratio of the irradiation modified attapulgite to the activated carbon to be 10:2, adding 50 mL of deionized water, uniformly mixing, stirring for 5h, adding 2g of acetic acid, placing in a muffle furnace, roasting at 500 ℃, and roasting for 30min to obtain the irradiation modified attapulgite/activated carbon composite material;
(3) and (3) mixing the irradiation modified attapulgite/activated carbon composite material obtained in the step (2) with a zinc oxide antibacterial agent according to a mass ratio of 1:5, adding a binder and a phosphate, mixing for 20 min at a speed of 30r/min by using a mixer, die-casting and molding, calcining for 1h at a high temperature of 650 ℃, and cooling to obtain the irradiation modified attapulgite composite carbon rod.
Measurement of Performance
Taking the irradiation modified attapulgite composite carbon rod prepared in example 1 as an example, the structural characteristics of the irradiation modified attapulgite and the adsorption performance of the composite carbon rod were measured.
(1) Scanning electron microscope
Sample morphology analysis using Scanning Electron Microscope (SEM)
FIG. 1 is an SEM image of attapulgite, which is seen to be closely packed in rod crystals; FIG. 2 is an SEM photograph of the acid-treated attapulgite in which the rod-crystal structure is opened and the inside of the attapulgite shows a porous structure; FIG. 3 is an SEM image of the radiation-modified attapulgite in which the compact rod-crystal structure is broken up and is in a loose state; fig. 4 is an SEM image of attapulgite modified by acid treatment and irradiation, which shows that the attapulgite modified by acid treatment and irradiation has a looser structure and exposes more pore structures, which contribute to the improvement of the adsorption capacity.
(2) Measurement of methyl blue adsorption Effect
Fig. 5 is a methyl blue adsorption effect graph (the initial concentration of methyl blue is 100mg/L), and the result shows that the irradiation modified attapulgite/activated carbon composite material prepared in this example 1 (i.e., acid + irradiation modified attapulgite/activated carbon in the graph) shows a better removal rate, the adsorption efficiency can reach 87.5% within 20 min, and the effect is superior to that of unmodified attapulgite composite activated carbon, acid modified attapulgite/activated carbon and irradiation modified attapulgite/activated carbon.
(3) Measurement of residual chlorine removal Effect
Fig. 6 is a graph showing residual chlorine removal effect (initial residual chlorine concentration of 10 mg/L), in which the ordinate represents residual chlorine removal rate and the abscissa represents time, and the results show that the irradiation-modified attapulgite/activated carbon composite material (i.e., acid + irradiation-modified attapulgite/activated carbon in the graph) prepared in example 1 exhibits a better chlorine removal rate. The composite material has high adsorption efficiency and fast rising speed within 60 min, and shows that the composite material has better effect than unmodified attapulgite composite activated carbon, acid modified attapulgite/activated carbon and irradiation modified attapulgite/activated carbon.
Claims (10)
1. A preparation method of an irradiation modified attapulgite/activated carbon composite carbon rod is characterized by comprising the following steps:
(1) dissolving attapulgite in water, carrying out acidification treatment, drying, grinding, placing on a high-energy electron beam irradiation conveyor belt, carrying out irradiation treatment, and grinding to obtain irradiation modified attapulgite;
(2) mixing the irradiation modified attapulgite with the activated carbon, dissolving in water, stirring uniformly, adding acetic acid, and roasting in a muffle furnace to obtain the irradiation modified attapulgite/activated carbon composite material;
(3) and (3) placing the irradiation modified attapulgite/activated carbon composite material obtained in the step (2), the zinc oxide antibacterial agent, the binder and the phosphate into a mixer to be uniformly mixed, die-casting and molding, calcining at high temperature, and cooling to obtain the irradiation modified attapulgite composite carbon rod.
2. The preparation method of the irradiation modified attapulgite/activated carbon composite carbon rod according to claim 1, wherein in the step (1), the reagent used for the acidification treatment is 1 ~ 2mol/L hydrochloric acid solution.
3. The preparation method of the irradiation modified attapulgite/activated carbon composite carbon rod according to claim 1, wherein in the step (1), the drying temperature is 60 ~ 80 ℃, and the drying time is 8 ~ 10 h.
4. The method for preparing the radiation modified attapulgite/activated carbon composite carbon rod according to claim 1, wherein in the step (1), the irradiation energy of the high-energy electron beam is 10 ~ 20MeV, and the irradiation dose is 30 ~ 50 KGy.
5. The preparation method of the irradiation modified attapulgite/activated carbon composite carbon rod as claimed in claim 1, wherein in the step (2), the stirring time is 5 ~ 6h, the roasting temperature is 400 ~ 500 ℃, and the roasting time is 30 ~ 50 min.
6. The preparation method of the irradiation modified attapulgite/activated carbon composite carbon rod as claimed in claim 1, wherein in the step (3), the mixing speed is 20 ~ 30r/min and the mixing time is 20 ~ 30 min.
7. The preparation method of the irradiation modified attapulgite/activated carbon composite carbon rod as claimed in claim 1, wherein in the step (3), the calcination temperature is 550 ~ 650 ℃ and the calcination time is 1 ~ 2 h.
8. The preparation method of the irradiation modified attapulgite/activated carbon composite carbon rod according to claim 1, wherein in the step (2), the mass ratio of the irradiation modified attapulgite to the activated carbon is 10 (1 ~ 3).
9. The preparation method of the irradiation modified attapulgite/activated carbon composite carbon rod according to claim 1, wherein in the step (3), the mass ratio of the zinc oxide antibacterial agent to the irradiation modified attapulgite/activated carbon composite material is (4 ~ 5): 1.
10. An irradiation modified attapulgite/active carbon composite carbon rod is characterized in that: prepared by the preparation method of the irradiation modified attapulgite/activated carbon composite carbon rod of any one of claims 1 to 9.
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Cited By (3)
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| CN112275039A (en) * | 2020-10-16 | 2021-01-29 | 安徽职业技术学院 | Purifying filter element and purifier comprising same |
| CN114606049A (en) * | 2022-03-21 | 2022-06-10 | 温州尚脉生物科技有限公司 | Preparation method of high-quality olive oil |
| CN115636495A (en) * | 2022-10-13 | 2023-01-24 | 淮阴工学院 | Preparation method of irradiation modified bentonite loaded vulcanized nano zero-valent iron |
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| CN115636495A (en) * | 2022-10-13 | 2023-01-24 | 淮阴工学院 | Preparation method of irradiation modified bentonite loaded vulcanized nano zero-valent iron |
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