CN110694592A - Sewage heavy metal ion plush type adsorbent and preparation method thereof - Google Patents

Sewage heavy metal ion plush type adsorbent and preparation method thereof Download PDF

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CN110694592A
CN110694592A CN201911076922.XA CN201911076922A CN110694592A CN 110694592 A CN110694592 A CN 110694592A CN 201911076922 A CN201911076922 A CN 201911076922A CN 110694592 A CN110694592 A CN 110694592A
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attapulgite
heavy metal
metal ion
plush
sewage
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张佳佳
陈迎
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Shunping Xuzhou Biotechnology Co Ltd
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Shunping Xuzhou Biotechnology Co Ltd
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/02Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
    • B01J20/10Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising silica or silicate
    • B01J20/12Naturally occurring clays or bleaching earth
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/22Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising organic material
    • B01J20/24Naturally occurring macromolecular compounds, e.g. humic acids or their derivatives
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/28Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
    • B01J20/28002Solid 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 physical properties
    • B01J20/28009Magnetic properties
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/28Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
    • B01J20/28014Solid 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
    • B01J20/28028Particles immobilised within fibres or filaments
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00Treatment of water, waste water, or sewage
    • C02F1/28Treatment of water, waste water, or sewage by sorption
    • C02F1/281Treatment of water, waste water, or sewage by sorption using inorganic sorbents
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00Treatment of water, waste water, or sewage
    • C02F1/28Treatment of water, waste water, or sewage by sorption
    • C02F1/286Treatment of water, waste water, or sewage by sorption using natural organic sorbents or derivatives thereof
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2101/00Nature of the contaminant
    • C02F2101/10Inorganic compounds
    • C02F2101/20Heavy metals or heavy metal compounds

Abstract

The invention discloses a sewage heavy metal ion plush type adsorbent and a preparation method thereof, belonging to the technical field of environmental protection, which can realize the activation modification of attapulgite by a way of first-later reaction of high-temperature steam and hydrochloric acid steam, increase the number of pore channels of the attapulgite, improve the specific surface area, increase the active space sites, greatly improve the adsorption capacity of the attapulgite in the heavy metal sewage, simultaneously uniformly disperse magnetic capture fibers into the activated and modified attapulgite for granulation molding under the assistance of a blowing device, distribute more magnetic capture fibers with loose surface and large specific surface area, are similar to plush-shaped adsorption balls, change the passive adsorption way of the traditional adsorbent, not only increase the contact area with the heavy metal ions through the magnetic capture fibers, improve the adsorption effect, but also play the active capture effect by utilizing the characteristic that the magnetic capture fibers can swing in the sewage, thereby obviously improving the adsorption treatment capability.

Description

Sewage heavy metal ion plush type adsorbent and preparation method thereof
Technical Field
The invention relates to the technical field of environmental protection, in particular to a sewage heavy metal ion plush type adsorbent and a preparation method thereof.
Background
The water environment is one of the basic elements constituting the environment, is an important place for the survival and development of the human society and is also the field which is most seriously interfered and damaged by human beings. The pollution and destruction of the aqueous environment has become one of the major environmental problems in the world today. Among them, heavy metal pollution is the most serious problem causing water environment pollution. Heavy metal pollution refers to environmental pollution caused by heavy metals or compounds thereof, and is mainly caused by human factors such as mining, waste gas emission, sewage irrigation, heavy metal product use and the like. Heavy metals are not easily dissolved and removed, and cannot be discharged after entering into living bodies, thereby causing chronic poisoning. Therefore, heavy metal pollution in the water environment not only causes great economic loss, but also seriously harms the health and survival of all organisms on the earth. Therefore, how to effectively solve the pollution of heavy metals to the water environment has become one of the hot spots of the research of governments and scholars of various countries in the world.
The heavy metals are different in type, different in valence state in nature, and different in treatment method. There are 3 common treatment methods: (1) the chemical treatment method, i.e., the method of removing heavy metal ions from wastewater by chemical reaction, is divided into a chemical precipitation method (neutralization precipitation method, sulfide precipitation method, ferrite precipitation method) and an electrochemical treatment method. (2) The physical treatment method refers to a method of adsorbing, concentrating and separating heavy metal ions in wastewater without changing their chemical forms, and includes ion exchange methods, electrodialysis methods, separation methods, solvent extraction methods, adsorption methods, and the like. (3) The biological treatment method is a method for removing heavy metal ions in wastewater by the action of flocculation, absorption accumulation, enrichment and the like of microorganisms or plants, and comprises a phytoremediation method, a biological flocculation method, a biological adsorption method and the like.
At present, the sewage treatment status of China mostly adopts the adsorbent in the physical treatment method, the treatment effect usually depends on the adsorption capacity of the adsorbent, the most common is activated carbon, however, the adsorption capacity of the existing activated carbon is effective, particularly, the adsorption activity is poor, the preparation cost is high, the regeneration is difficult, the desorption is difficult after the adsorption saturation, the water treatment cost is high due to the fact that most of the activated carbon is directly scrapped, and the development of the physical treatment of the sewage polluted by heavy metal is restricted.
Disclosure of Invention
1. Technical problem to be solved
Aiming at the problems in the prior art, the invention aims to provide a sewage heavy metal ion plush adsorbent and a preparation method thereof, which can activate and modify attapulgite in a high-temperature steam and hydrochloric acid steam first-after reaction mode, increase the number of pore channels of the attapulgite, increase the specific surface area, increase active space sites, greatly improve the adsorption capacity of the attapulgite in heavy metal sewage, uniformly disperse magnetic capture fibers into the activated and modified attapulgite with the assistance of a blowing device for granulation and molding, distribute more magnetic capture fibers with loose surface and large specific surface area and also distribute more magnetic capture and paving fibers similar to plush adsorption balls, change the passive adsorption mode of the traditional adsorbent, increase the contact area with heavy metal ions through the magnetic capture and paving fibers, improve the adsorption effect, and play the active capture effect by utilizing the characteristic that the magnetic capture and paving fibers can swing in sewage, thereby obviously improving the adsorption treatment capacity, realizing recovery by acid washing after adsorption saturation, having low cost and good effect.
2. Technical scheme
In order to solve the above problems, the present invention adopts the following technical solutions.
A sewage heavy metal ion plush type adsorbent comprises the following components in parts by weight: 40-60 parts of attapulgite, 20-30 parts of magnetic capture fiber, 0.1-1 part of dispersant, 70-80 parts of deionized water, 5-10 parts of hydrochloric acid solution, 1-10 parts of adhesive and 15-20 parts of chitosan.
Furthermore, the magnetic capture fiber is prepared by immersing superfine fibers with the length of 0.1-1mm and the diameter of 0.5-5 mu m in a magnetic fluid, standing for 2h, taking out and drying at 60-80 ℃, has the adsorption characteristic of the superfine fibers, can effectively capture tiny pollutants and heavy metals, has high strength and toughness, is not easy to break, and is convenient for technicians to directly recover by using a magnetic field after magnetism.
Further, sodium hexametaphosphate or sodium orthophosphate is adopted as the dispersing agent.
Furthermore, the concentration of the hydrochloric acid solution is 36% -38%, the hydrochloric acid solution can dissolve part of the attapulgite structure, the undissolved part plays a supporting role, the number of the pore channels is increased, the specific surface area is increased, meanwhile, the attapulgite pore channels often contain impurities such as carbonate, and the impurities distributed in the attapulgite pore channels can be removed through acidification treatment, so that the pore channels are dredged to enhance the permeability; on the other hand, due to the cation exchangeability of attapulgite, H + having a small radius can displace plasma such as Kt, Nat, Ca and Mg in the interlaminar portion of attapulgite, increasing the pore volume and enhancing the adsorption performance.
Further, the adhesive is polyvinyl alcohol aqueous solution, paraffin, novolac or sulfurous acid pulp waste liquid.
A preparation method of a sewage heavy metal ion plush type adsorbent comprises the following steps:
s1, purifying the attapulgite into a fine powder material with 500 meshes by washing, drying, crushing and sieving pretreatment measures, then mixing the attapulgite with deionized water, dropwise adding a small amount of dispersant, stirring, standing, filtering and drying;
s2, heating the attapulgite prepared by drying in the step S1 from room temperature to 250 ℃, using inert gas nitrogen as carrier gas to enable water vapor to contact and react with the attapulgite, further heating to 350 ℃ for 1-2h, introducing hydrochloric acid vapor for 5-10min and beginning to cool, stopping adding the water vapor, taking out the attapulgite after the temperature is cooled to room temperature, and washing the attapulgite with absolute ethyl alcohol and deionized water one time;
s3, mixing the magnetic capture fiber and the adhesive in advance through a blowing device, adding the mixture into the attapulgite prepared in the step S2, putting the mixture into a granulator, gradually adding chitosan during granulation, and granulating to obtain a granular adsorbent with the particle size of 0.1-1 mm;
s4, roasting the granular adsorbent obtained in the step S3 at the high temperature of 350-450 ℃ under the protection of nitrogen for 2-5h to remove crystal water, and sealing and storing to obtain the plush-like adsorbent.
Further, the flow rate of the water vapor in the step S2 is controlled to be 1L-5L/h, the flow rate of the hydrochloric acid vapor is controlled to be 0.5-1L/h, the water vapor flow rate is high to play a role of quick impact, the porosity and the specific surface area of the attapulgite are improved, and the slow flow rate of the hydrochloric acid vapor can have sufficient reaction time to dissolve the attapulgite.
Further, blow off the device and include the working plate, working plate upper end fixedly connected with installing support, working plate upper end fixedly connected with slide rail, sliding connection has the slider on the slide rail, slider upper end fixedly connected with holds the thing shell, install electric putter on the installing support, and electric putter's extension end with hold thing shell fixed connection, it is equipped with the interpolation pipe to hold thing shell upside, and adds fixed connection between pipe and the installing support, add the mixed funnel that pipe upper end fixedly connected with is linked together, add and install the valve on the pipe.
Furthermore, add the outside of tubes end and install electronic air pump, the air-out end of electronic air pump is connected with the hard tube of blowing, and the hard tube of blowing stretches into from adding the pipe lower extreme, the dispersion spherical shell that the hard tube upper end fixedly connected with of blowing is linked together, it has a plurality of evenly distributed's dispersion gas pocket to cut on the dispersion spherical shell.
Further, in the step S4, the temperature rising rate of the roasting temperature is kept at a constant temperature of 10 ℃/min to 350 ℃ and 450 ℃, air cooling is carried out to the room temperature after the roasting is finished, and the temperature is raised at a relatively slow speed to avoid that the collapse stability of the internal structure is reduced due to severe water loss of the attapulgite.
3. Advantageous effects
Compared with the prior art, the invention has the advantages that:
the scheme can realize activation modification of the attapulgite by a mode of first-later reaction of high-temperature steam and hydrochloric acid steam, increase the number of pore passages of the attapulgite, improve the specific surface area, increase active space sites, greatly improve the adsorption capacity of the attapulgite in heavy metal sewage, simultaneously uniformly disperse magnetic capture fibers into the attapulgite after activation modification under the assistance of a blowing device for granulation and molding, distribute more magnetic capture fibers similar to plush-shaped adsorption balls while having larger surface porous specific surface area, change the passive adsorption mode of the traditional adsorbent, increase the contact area with heavy metal ions by the magnetic capture fibers, improve the adsorption effect, play the active capture effect by utilizing the characteristic that the magnetic capture fibers can swing in the sewage, thereby obviously improving the adsorption capacity and treatment, realize recovery by acid washing after adsorption saturation, low cost and good effect.
Drawings
FIG. 1 is a table of the composition of the present invention;
FIG. 2 is a schematic structural view of the present invention;
FIG. 3 is a schematic structural diagram of a blowing device according to the present invention;
FIG. 4 is a schematic structural view of the magnetic capture fiber of the present invention in a blown-off state;
FIG. 5 is a flow chart of the preparation of the present invention.
The reference numbers in the figures illustrate:
the device comprises a working plate 1, a mounting bracket 2, an adding pipe 3, a sliding rail 4, a sliding block 5, an object bearing shell 6, an electric push rod 7, a mixing funnel 8, an electric air pump 9, an air blowing hard pipe 10, a dispersing spherical shell 11 and a dispersing air hole 12.
Detailed Description
The technical solution in the embodiments of the present invention will be clearly and completely described below with reference to the accompanying drawings in the embodiments of the present invention; it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments, and all other embodiments obtained by those skilled in the art without any inventive work are within the scope of the present invention.
In the description of the present invention, it should be noted that the terms "upper", "lower", "inner", "outer", "top/bottom", and the like indicate orientations or positional relationships based on those shown in the drawings, and are only for convenience of description and simplification of description, but do not indicate or imply that the referred device or element must have a specific orientation, be constructed in a specific orientation, and be operated, and thus should not be construed as limiting the present invention. Furthermore, the terms "first" and "second" are used for descriptive purposes only and are not to be construed as indicating or implying relative importance.
In the description of the present invention, it should be noted that, unless otherwise specifically stated or limited, the terms "mounted," "disposed," "sleeved/connected," "connected," and the like are used in a broad sense, and for example, "connected" may be a fixed connection, a detachable connection, an integral connection, a mechanical connection, an electrical connection, a direct connection, an indirect connection through an intermediate medium, and a communication between two elements.
Example 1:
referring to fig. 1, a sewage heavy metal ion plush type adsorbent comprises the following components in parts by weight: 40 parts of attapulgite, 20 parts of magnetic capture fiber, 0.1 part of dispersant, 70 parts of deionized water, 5 parts of hydrochloric acid solution, 1 part of adhesive and 15 parts of chitosan.
The magnetic capture fiber is prepared by soaking superfine fiber with the length of 0.1-1mm and the diameter of 0.5-5 mu m in a magnetic fluid, standing for 2h, taking out and drying at 60-80 ℃, has the adsorption characteristic of the superfine fiber, can effectively capture tiny pollutants and heavy metals, has high strength and high toughness, is not easy to break, and is convenient for technicians to directly recover by using a magnetic field after magnetism.
The dispersing agent adopts sodium hexametaphosphate or sodium orthophosphate.
The concentration of the hydrochloric acid solution is 36% -38%, the hydrochloric acid solution can dissolve part of the attapulgite structure, the undissolved part plays a supporting role, the number of the pore passages is increased, the specific surface area is increased, meanwhile, the attapulgite pore passages often contain impurities such as carbonate, and the impurities distributed in the attapulgite pore passages can be removed through acidification treatment, so that the pore passages are dredged and the permeability is enhanced; on the other hand, due to the cation exchangeability of attapulgite, H + having a small radius can displace plasma such as Kt, Nat, Ca and Mg in the interlaminar portion of attapulgite, increasing the pore volume and enhancing the adsorption performance.
The adhesive is polyvinyl alcohol aqueous solution, paraffin, novolac or sulfurous acid pulp waste liquid.
Referring to fig. 5, a method for preparing a sewage heavy metal ion plush type adsorbent includes the following steps:
s1, purifying the attapulgite into a fine powder material with 500 meshes by washing, drying, crushing and sieving pretreatment measures, then mixing the attapulgite with deionized water, dropwise adding a small amount of dispersant, stirring, standing, filtering and drying;
s2, heating the attapulgite prepared by drying in the step S1 from room temperature to 250 ℃, using inert gas nitrogen as carrier gas to enable water vapor to contact and react with the attapulgite, further heating to 300 ℃, keeping for 1h, introducing hydrochloric acid vapor for 5min, starting cooling, stopping adding the water vapor, taking out the attapulgite after the temperature is reduced to the room temperature, and washing the attapulgite with absolute ethyl alcohol and deionized water one time;
s3, mixing the magnetic capture fiber and the adhesive in advance through a blowing device, adding the mixture into the attapulgite prepared in the step S2, putting the mixture into a granulator, gradually adding chitosan during granulation, and granulating to obtain a granular adsorbent with the particle size of 0.1-1 mm;
and S4, roasting the granular adsorbent obtained in the step S3 at the high temperature of 350 ℃ under the protection of nitrogen for 2 hours to remove crystal water, and sealing and storing the granular adsorbent to obtain the plush-like adsorbent with reference to the figure 2.
The flow rate of the water vapor in the step S2 is controlled to be 1L-5L/h, the flow rate of the hydrochloric acid vapor is controlled to be 0.5-1L/h, the water vapor flow rate is high, the rapid impact effect is achieved, the porosity and the specific surface area of the attapulgite are improved, and the sufficient reaction time can be provided for dissolving the attapulgite when the hydrochloric acid vapor flow rate is low.
Referring to fig. 3-4, the blowing device includes a working plate 1, an installation support 2 is fixedly connected to the upper end of the working plate 1, a slide rail 4 is fixedly connected to the upper end of the working plate 1, a slide block 5 is slidably connected to the slide rail 4, an object bearing housing 6 is fixedly connected to the upper end of the slide block 5, an electric push rod 7 is installed on the installation support 2, an extension end of the electric push rod 7 is fixedly connected to the object bearing housing, an adding pipe 3 is disposed on the upper side of the object bearing housing 6, the adding pipe 3 is fixedly connected to the installation support 2, the adding pipe 3 provides an input channel for magnetically capturing fibers, a mixing funnel 8 is fixedly connected to the upper end of the adding pipe 3 for providing a mixing space for magnetically capturing fibers and an adhesive, a valve is installed on the adding pipe 3 for controlling the opening and closing of the adding pipe 3, an electric air pump 9 is installed at the outer end of the adding pipe 3, the blowing hard tube 10 extends into the lower end of the adding tube 3, the upper end of the blowing hard tube 10 is fixedly connected with a dispersing spherical shell 11 which is communicated with each other, the dispersing spherical shell 11 plays a role in preliminarily dispersing and separating the magnetic capture fibers so as to disperse the magnetic capture fibers along the circumferential direction, the problem that the magnetic capture fibers are connected together due to the magnetic adsorption relation to influence the distribution effect of the magnetic capture fibers after subsequent granulation is avoided, a plurality of uniformly distributed dispersing air holes 12 are drilled in the dispersing spherical shell 11 to play a role in secondarily dispersing the magnetic capture fibers, and the magnetic capture fibers which are connected together or wound together are blown by wind power so as to be scattered to fall on the attapulgite in the object bearing shell 6.
When in use, the activated and modified attapulgite is flatly laid in the object bearing shell 6, the magnetic catching fibers and the adhesive are mixed in the mixing funnel 8, then the valve is opened, the magnetic catching fibers fall from the adding pipe 3 and are dispersed for the first time when passing through the dispersing spherical shell 11, then the magnetic catching fibers are blown out from the dispersing air holes 12 by wind power provided by the electric air pump 9 to be dispersed for the second time, the dispersed magnetic catching fibers fall on the attapulgite, and are temporarily adhered to the attapulgite without conglomeration and winding due to the action of the adhesive, meanwhile, the electric push rod 7 pushes the object bearing shell 6 to move left, so that the magnetic catching fibers falling all the time are uniformly dispersed and added on the tiled attapulgite, the magnetic catching fibers are positioned after contacting with the attapulgite under the action of the adhesive, and cannot be mutually attracted and wound, so that the magnetic catching fibers can be uniformly and orderly distributed on the granulated attapulgite.
In the step S4, the temperature rising rate of the roasting temperature is kept at 10 ℃/min to 350-.
Example 2:
referring to fig. 1, a sewage heavy metal ion plush type adsorbent comprises the following components in parts by weight: 60 parts of attapulgite, 30 parts of magnetic capture fiber, 1 part of dispersant, 80 parts of deionized water, 10 parts of hydrochloric acid solution, 10 parts of adhesive and 20 parts of chitosan.
A preparation method of a sewage heavy metal ion plush type adsorbent comprises the following steps:
s1, purifying the attapulgite into a fine powder material with 500 meshes by washing, drying, crushing and sieving pretreatment measures, then mixing the attapulgite with deionized water, dropwise adding a small amount of dispersant, stirring, standing, filtering and drying;
s2, heating the attapulgite prepared by drying in the step S1 from room temperature to 250 ℃, using inert gas nitrogen as carrier gas to enable water vapor to contact and react with the attapulgite, further heating to 350 ℃, keeping for 2h, introducing hydrochloric acid vapor for 10min, starting cooling, stopping adding the water vapor, taking out the attapulgite after the temperature is reduced to the room temperature, and washing the attapulgite with absolute ethyl alcohol and deionized water one time;
s3, mixing the magnetic capture fiber and the adhesive in advance through a blowing device, adding the mixture into the attapulgite prepared in the step S2, putting the mixture into a granulator, gradually adding chitosan during granulation, and granulating to obtain a granular adsorbent with the particle size of 0.1-1 mm;
and S4, roasting the granular adsorbent obtained in the step S3 at the high temperature of 450 ℃ under the protection of nitrogen for 5 hours to remove crystal water, and sealing and storing the granular adsorbent to obtain the plush-like adsorbent with reference to the figure 2.
The remainder was in accordance with example 1.
Example 3:
referring to fig. 1, a sewage heavy metal ion plush type adsorbent comprises the following components in parts by weight: 50 parts of attapulgite, 25 parts of magnetic capture fiber, 0.5 part of dispersant, 75 parts of deionized water, 8 parts of hydrochloric acid solution, 5 parts of adhesive and 18 parts of chitosan.
A preparation method of a sewage heavy metal ion plush type adsorbent comprises the following steps:
s1, purifying the attapulgite into a fine powder material with 500 meshes by washing, drying, crushing and sieving pretreatment measures, then mixing the attapulgite with deionized water, dropwise adding a small amount of dispersant, stirring, standing, filtering and drying;
s2, heating the attapulgite prepared by drying in the step S1 from room temperature to 250 ℃, using inert gas nitrogen as carrier gas to enable water vapor to contact and react with the attapulgite, further heating to 330 ℃, keeping for 1.5h, introducing hydrochloric acid vapor for 8min, starting cooling, stopping adding the water vapor, taking out the attapulgite after the temperature is reduced to the room temperature, and washing the attapulgite with absolute ethyl alcohol and deionized water successively;
s3, mixing the magnetic capture fiber and the adhesive in advance through a blowing device, adding the mixture into the attapulgite prepared in the step S2, putting the mixture into a granulator, gradually adding chitosan during granulation, and granulating to obtain a granular adsorbent with the particle size of 0.1-1 mm;
and S4, roasting the granular adsorbent obtained in the step S3 at a high temperature of 400 ℃ under the protection of nitrogen for 3 hours to remove crystal water, and sealing and storing the granular adsorbent with reference to the figure 2 to obtain the plush-like adsorbent.
The remainder was in accordance with example 1.
The invention can realize activation modification of the attapulgite by a mode of first-later reaction of high-temperature steam and hydrochloric acid steam, increase the number of pore passages of the attapulgite, improve the specific surface area, increase active space sites, greatly improve the adsorption capacity of the attapulgite in heavy metal sewage, simultaneously uniformly disperse magnetic capture fibers into the attapulgite after activation modification under the assistance of a blowing device for granulation and molding, and the attapulgite with a loose surface, a plurality of pores and a larger specific surface area is also distributed with magnetic capture fibers which are similar to plush adsorption balls, thereby changing the passive adsorption mode of the traditional adsorbent, increasing the contact area with heavy metal ions by the magnetic capture fibers, improving the adsorption effect, and simultaneously playing the active capture effect by utilizing the characteristic that the attapulgite can swing in the sewage, thereby obviously improving the adsorption treatment capacity, and realizing recovery by acid washing after adsorption saturation, low cost and good effect.
The foregoing is only a preferred embodiment of the present invention; the scope of the invention is not limited thereto. Any person skilled in the art should be able to cover the technical scope of the present invention by equivalent or modified solutions and modifications within the technical scope of the present invention.

Claims (10)

1. The sewage heavy metal ion plush type adsorbent is characterized in that: the paint comprises the following components in parts by weight: 40-60 parts of attapulgite, 20-30 parts of magnetic capture fiber, 0.1-1 part of dispersant, 70-80 parts of deionized water, 5-10 parts of hydrochloric acid solution, 1-10 parts of adhesive and 15-20 parts of chitosan.
2. The sewage heavy metal ion plush type adsorbent as claimed in claim 1, wherein: the magnetic catching fiber is prepared by soaking superfine fiber with the length of 0.1-1mm and the diameter of 0.5-5 mu m in magnetic fluid, standing for 2h, taking out, and drying at 60-80 ℃.
3. The sewage heavy metal ion plush type adsorbent as claimed in claim 1, wherein: the dispersing agent adopts sodium hexametaphosphate or sodium orthophosphate.
4. The sewage heavy metal ion plush type adsorbent as claimed in claim 1, wherein: the concentration of the hydrochloric acid solution is 36-38%.
5. The sewage heavy metal ion plush type adsorbent as claimed in claim 1, wherein: the adhesive is polyvinyl alcohol aqueous solution, paraffin, novolac or sulfurous acid pulp waste liquid.
6. The method for preparing the sewage heavy metal ion plush type adsorbent according to any one of the claims 1 to 5, characterized in that: the method comprises the following steps:
s1, purifying the attapulgite into a fine powder material with 500 meshes by washing, drying, crushing and sieving pretreatment measures, then mixing the attapulgite with deionized water, dropwise adding a small amount of dispersant, stirring, standing, filtering and drying;
s2, heating the attapulgite prepared by drying in the step S1 from room temperature to 250 ℃, using inert gas nitrogen as carrier gas to enable water vapor to contact and react with the attapulgite, further heating to 350 ℃ for 1-2h, introducing hydrochloric acid vapor for 5-10min and beginning to cool, stopping adding the water vapor, taking out the attapulgite after the temperature is cooled to room temperature, and washing the attapulgite with absolute ethyl alcohol and deionized water one time;
s3, mixing the magnetic capture fiber and the adhesive in advance through a blowing device, adding the mixture into the attapulgite prepared in the step S2, putting the mixture into a granulator, gradually adding chitosan during granulation, and granulating to obtain a granular adsorbent with the particle size of 0.1-1 mm;
s4, roasting the granular adsorbent obtained in the step S3 at the high temperature of 350-450 ℃ under the protection of nitrogen for 2-5h to remove crystal water, and sealing and storing to obtain the plush-like adsorbent.
7. The preparation method of the sewage heavy metal ion plush type adsorbent according to the claim 6, characterized in that: the flow rate of the water vapor in the step S2 is controlled to be 1L-5L/h, and the flow rate of the hydrochloric acid vapor is controlled to be 0.5-1L/h.
8. The preparation method of the sewage heavy metal ion plush type adsorbent according to the claim 6, characterized in that: blow the device and include working plate (1), working plate (1) upper end fixedly connected with installing support (2), working plate (1) upper end fixedly connected with slide rail (4), sliding connection has slider (5) on slide rail (4), slider (5) upper end fixedly connected with holds thing shell (6), install electric putter (7) on installing support (2), and the extension end of electric putter (7) with hold thing shell fixed connection, it is equipped with interpolation pipe (3) to hold thing shell (6) upside, and adds fixed connection between pipe (3) and installing support (2), add mixed funnel (8) that pipe (3) upper end fixedly connected with is linked together, install the valve on adding pipe (3).
9. The preparation method of the sewage heavy metal ion plush type adsorbent according to the claim 8, characterized in that: add pipe (3) outer end and install electronic air pump (9), the air-out end of electronic air pump (9) is connected with the hard tube (10) of blowing, and blows hard tube (10) and stretch into from adding pipe (3) lower extreme, the dispersion spherical shell (11) that the hard tube (10) upper end fixedly connected with of blowing is linked together, cut dispersed gas pocket (12) that have a plurality of evenly distributed on dispersion spherical shell (11).
10. The preparation method of the sewage heavy metal ion plush type adsorbent according to the claim 6, characterized in that: in the step S4, the temperature rising rate of the roasting temperature is kept at a constant temperature of 10 ℃/min to 350-450 ℃, and after the roasting is finished, the air is cooled to the room temperature.
CN201911076922.XA 2019-11-06 2019-11-06 Sewage heavy metal ion plush type adsorbent and preparation method thereof Withdrawn CN110694592A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112619360A (en) * 2020-05-08 2021-04-09 黄龙标 Unitized self-cleaning type filtering method for organic waste gas treatment

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112619360A (en) * 2020-05-08 2021-04-09 黄龙标 Unitized self-cleaning type filtering method for organic waste gas treatment

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