CN115075055B - Nano magnetic oxide composite tea paper and preparation method thereof - Google Patents

Nano magnetic oxide composite tea paper and preparation method thereof Download PDF

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CN115075055B
CN115075055B CN202210679798.1A CN202210679798A CN115075055B CN 115075055 B CN115075055 B CN 115075055B CN 202210679798 A CN202210679798 A CN 202210679798A CN 115075055 B CN115075055 B CN 115075055B
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magnetic oxide
nano
tea
oxide composite
tea paper
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CN115075055A (en
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于刚
刁瑞雪
张学志
车蒙阳
王亚宁
杨俊�
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Shijiazhuang Tiedao University
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Shijiazhuang Tiedao University
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    • D—TEXTILES; PAPER
    • D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
    • D21H—PULP COMPOSITIONS; PREPARATION THEREOF NOT COVERED BY SUBCLASSES D21C OR D21D; IMPREGNATING OR COATING OF PAPER; TREATMENT OF FINISHED PAPER NOT COVERED BY CLASS B31 OR SUBCLASS D21G; PAPER NOT OTHERWISE PROVIDED FOR
    • D21H27/00—Special paper not otherwise provided for, e.g. made by multi-step processes
    • 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
    • B01J20/06—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising oxides or hydroxides of metals not provided for in group B01J20/04
    • 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
    • B01J20/28002—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 physical properties
    • B01J20/28009—Magnetic properties
    • 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
    • B01J20/28033—Membrane, sheet, cloth, pad, lamellar or mat
    • 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
    • B01J20/28054—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 surface properties or porosity
    • B01J20/28057—Surface area, e.g. B.E.T specific surface area
    • B01J20/28061—Surface area, e.g. B.E.T specific surface area being in the range 100-500 m2/g
    • 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
    • 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
    • D—TEXTILES; PAPER
    • D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
    • D21H—PULP COMPOSITIONS; PREPARATION THEREOF NOT COVERED BY SUBCLASSES D21C OR D21D; IMPREGNATING OR COATING OF PAPER; TREATMENT OF FINISHED PAPER NOT COVERED BY CLASS B31 OR SUBCLASS D21G; PAPER NOT OTHERWISE PROVIDED FOR
    • D21H11/00—Pulp or paper, comprising cellulose or lignocellulose fibres of natural origin only
    • D21H11/12—Pulp from non-woody plants or crops, e.g. cotton, flax, straw, bagasse
    • D—TEXTILES; PAPER
    • D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
    • D21H—PULP COMPOSITIONS; PREPARATION THEREOF NOT COVERED BY SUBCLASSES D21C OR D21D; IMPREGNATING OR COATING OF PAPER; TREATMENT OF FINISHED PAPER NOT COVERED BY CLASS B31 OR SUBCLASS D21G; PAPER NOT OTHERWISE PROVIDED FOR
    • D21H17/00—Non-fibrous material added to the pulp, characterised by its constitution; Paper-impregnating material characterised by its constitution
    • D21H17/20—Macromolecular organic compounds
    • D21H17/21—Macromolecular organic compounds of natural origin; Derivatives thereof
    • D21H17/24—Polysaccharides
    • D21H17/25—Cellulose
    • D—TEXTILES; PAPER
    • D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
    • D21H—PULP COMPOSITIONS; PREPARATION THEREOF NOT COVERED BY SUBCLASSES D21C OR D21D; IMPREGNATING OR COATING OF PAPER; TREATMENT OF FINISHED PAPER NOT COVERED BY CLASS B31 OR SUBCLASS D21G; PAPER NOT OTHERWISE PROVIDED FOR
    • D21H17/00—Non-fibrous material added to the pulp, characterised by its constitution; Paper-impregnating material characterised by its constitution
    • D21H17/20—Macromolecular organic compounds
    • D21H17/21—Macromolecular organic compounds of natural origin; Derivatives thereof
    • D21H17/24—Polysaccharides
    • D21H17/28—Starch
    • D—TEXTILES; PAPER
    • D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
    • D21H—PULP COMPOSITIONS; PREPARATION THEREOF NOT COVERED BY SUBCLASSES D21C OR D21D; IMPREGNATING OR COATING OF PAPER; TREATMENT OF FINISHED PAPER NOT COVERED BY CLASS B31 OR SUBCLASS D21G; PAPER NOT OTHERWISE PROVIDED FOR
    • D21H17/00—Non-fibrous material added to the pulp, characterised by its constitution; Paper-impregnating material characterised by its constitution
    • D21H17/63—Inorganic compounds
    • D21H17/67—Water-insoluble compounds, e.g. fillers, pigments
    • D21H17/675—Oxides, hydroxides or carbonates
    • D—TEXTILES; PAPER
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    • D21H—PULP COMPOSITIONS; PREPARATION THEREOF NOT COVERED BY SUBCLASSES D21C OR D21D; IMPREGNATING OR COATING OF PAPER; TREATMENT OF FINISHED PAPER NOT COVERED BY CLASS B31 OR SUBCLASS D21G; PAPER NOT OTHERWISE PROVIDED FOR
    • D21H21/00—Non-fibrous material added to the pulp, characterised by its function, form or properties; Paper-impregnating or coating material, characterised by its function, form or properties
    • D21H21/50—Non-fibrous material added to the pulp, characterised by its function, form or properties; Paper-impregnating or coating material, characterised by its function, form or properties characterised by form
    • D21H21/52—Additives of definite length or shape
    • 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
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
    • Y02W10/00—Technologies for wastewater treatment
    • Y02W10/10—Biological treatment of water, waste water, or sewage

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Abstract

The invention discloses a nano magnetic oxide composite tea paper and a preparation method thereof. The preparation method combines the atomization spraying and the freeze drying to compound the nanometer magnetic oxide on the tea paper carrier evenly, quickly and efficiently, avoids the agglomeration of the nanometer particles of the magnetic oxide, fully utilizes the high specific surface area of the tea, and improves the quality of the nanometer magnetic oxide in the compound tea paper; the silane coupling agent has a good auxiliary effect on improving the bonding strength of the nano magnetic oxide and the tea paper carrier, so that the loss of the magnetic oxide in the using process can be avoided, and the prepared nano magnetic oxide composite tea paper not only has outstanding adsorption capacity, but also has good recycling performance.

Description

Nano magnetic oxide composite tea paper and preparation method thereof
Technical Field
The invention belongs to the technical field of sewage treatment, and particularly relates to nano magnetic oxide composite tea paper and a preparation method thereof.
Background
In the field of heavy metal ion wastewater treatment, an adsorption method is a simple and efficient treatment technology. Tea is an ideal biological treatment material, the net porous structure of the tea enables the tea to have a large specific surface area, and the tea polyphenol substances in the tea contain a large amount of active groups such as hydroxyl groups, amino groups and the like, and the active groups can exchange or combine with metal ions. Therefore, the tea has important application value in the field of heavy metal wastewater treatment.
But because reasons such as self size, tealeaves class adsorbent is mostly powdered or graininess, lose easily and be difficult to the recovery in the use, and in the practical application in-process, tealeaves class adsorbent breeds the bacterium easily and to the absorption of heavy metal ion and combine reasons such as stability relatively poor, lead to tealeaves class adsorbent to release a small amount of adsorbed heavy metal ion easily in adsorption process, cause secondary pollution, consequently how to handle tealeaves effectively, make tealeaves can obtain better application in heavy metal ion waste water treatment field in-process, be a research direction in heavy metal waste water treatment field.
Disclosure of Invention
The invention provides a nano magnetic oxide composite tea paper and a preparation method thereof, aiming at the technical problems existing in the application of tea in the field of heavy metal ion wastewater treatment in the prior art.
In order to achieve the purpose of the invention, the embodiment of the invention adopts the following technical scheme:
a preparation method of nano magnetic oxide composite tea paper specifically comprises the following steps:
s1: adding an alkali metal hydroxide solution into the boiled and stemmed tea leaves for soaking, adding citric acid to adjust the pH value to 6 to 8, and carrying out solid-liquid separation to obtain pretreated tea leaves;
s2: mixing the pretreated tea leaves obtained in the step S1 with water, a starch binder and cellulose fibers, adjusting the solid content of the mixed solution to 3-5%, and grinding to obtain slurry;
s3: removing water from the slurry obtained in the step S2, then, sheet making, forming and drying to obtain a tea paper carrier;
s4: and (2) adding a silane coupling agent into an aqueous dispersion liquid of the nano magnetic oxide with the mass fraction of 20-40%, atomizing and spraying the aqueous dispersion liquid to the tea paper carrier obtained in the step (S3), and freeze-drying at the temperature of-20 to-10 ℃ and in an environment of 4 to 6Pa to obtain the nano magnetic oxide composite tea paper.
Compared with the prior art, the preparation method of the nano magnetic oxide composite tea paper provided by the invention has the advantages that firstly, lignin in tea is destroyed by adding sodium hydroxide after boiling, the pore structure of tea fibers is fully improved, and a solid foundation is laid for the flexibility of a tea paper carrier obtained by subsequent preparation; then, the nano magnetic oxide is uniformly and efficiently compounded on the tea paper carrier in a mode of combining atomization spraying with freeze drying, so that the agglomeration of the nano ions of the magnetic oxide is avoided, the high specific surface area of the tea is fully utilized, and the quality of the nano magnetic oxide in the composite tea paper is improved; the silane coupling agent has a good auxiliary effect on improving the bonding strength of the nano magnetic oxide and the tea paper carrier, and can avoid the loss of the magnetic oxide in the using process, so that the prepared nano magnetic oxide composite tea paper not only has outstanding adsorption capacity, but also has good recycling performance.
Preferably, the mass ratio of the tea leaves pretreated in the S2 to water, starch binder and cellulose fibers is 1:30 to 50:0.01 to 0.06:0.05 to 0.2.
The optimized mass ratio of the tea leaves to the water, the starch binder and the cellulose fibers can ensure the quality of the tea paper carrier, so that the tea paper carrier has excellent mechanical properties and the porosity of the tea paper is improved to more than 70%.
Preferably, the particle diameter of the magnetic oxide in the aqueous dispersion of the nano magnetic oxide is 30 to 50nm.
Preferably, the magnetic oxide is at least one of ferroferric oxide and tricobalt tetroxide.
Preferably, the first and second electrodes are formed of a metal, the silane coupling agent is an epoxy silane coupling agent; the mass fraction of the silane coupling agent in the S4 in the nano magnetic oxide aqueous dispersion liquid is 0.3-0.5%.
The epoxy silane coupling agent has better stability in the system of the scheme, can further improve the composite effect of the metal oxide and the tea paper carrier, and prolongs the service life of the composite tea paper.
Preferably, the mass fraction of the sodium hydroxide solution in S1 is 1.9 to 2.5 percent, 20 to 40ml of the sodium hydroxide solution is added into each gram of tea, and the soaking treatment time after the sodium hydroxide solution is added is 6 to 12h.
The invention also provides nano magnetic oxide composite tea paper, which is prepared by adopting the preparation method of the nano magnetic oxide composite tea paper, and has the thickness of 0.8-1.2mm, the porosity of 70-90 percent and the mass per unit area of 100-120g/m 2 。
Preferably, the particle size of the nano magnetic oxide in the nano magnetic oxide composite tea paper is 30 to 50nm.
Drawings
In order to more clearly illustrate the technical solution in the embodiments of the present invention, the drawings required to be used in the embodiments will be briefly described below.
FIG. 1 is an optical photograph of a tea sheet prepared in example 1 of the present invention;
FIG. 2 is an optical photograph of the nano-magnetic oxide composite tea paper prepared in example 1 of the present invention;
FIG. 3 is a schematic diagram of the mechanical properties of the nano-magnetic oxide composite tea paper prepared in example 1 of the present invention;
FIG. 4 is an SEM image of the nano-magnetic oxide composite tea paper prepared in example 1 of the present invention;
fig. 5 is an XRD chart of the nano magnetic oxide composite tea paper prepared in example 1 of the present invention.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is further described in detail with reference to the following embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and do not limit the invention.
Example 1
The embodiment provides a nano ferroferric oxide composite tea paper and a preparation method thereof, and the preparation method of the nano ferroferric oxide composite tea paper comprises the following steps:
s1: adding 200ml of sodium hydroxide solution with solute mass fraction of 2.0% into 8g of boiled and stemmed tea leaves, soaking for 10 hours, adding citric acid to adjust the pH value to 7, filtering, washing with water, and drying to obtain pretreated tea leaves;
s2: mixing the pretreated tea leaves obtained in the step S1 with water, a starch binder and cellulose fibers, adjusting the mixed solid content to 4%, and grinding to obtain slurry, wherein the mass ratio of the treated tea leaves to the water, the starch binder and the cellulose fibers is 1:40:0.03:0.1;
s3: pouring the slurry obtained in the step S2 into a paper liquid former, carrying out vacuum suction filtration to remove water, forming sheets, and drying at 100 ℃ to obtain a tea paper carrier;
s4: adding a silane coupling agent into a nano ferroferric oxide aqueous nano dispersion liquid with the mass fraction of 20% and the nano ferroferric oxide particle size of 30 to 50nm, controlling the mass fraction of the silane coupling agent in the dispersion liquid to be 0.3%, atomizing and spraying the mixture to the tea paper carrier obtained in the step S3, and freeze-drying the tea paper carrier at the temperature of-15 ℃ and the pressure of 5Pa to obtain the nano ferroferric oxide composite tea paper, wherein the pressure of compressed gas in the atomizing and spraying process is 30psi, and the silane coupling agent is KH-560.
Through the inspection: the tea paper has thickness of 1.0mm, porosity of 85%, and mass per unit area of 115g/m 2 。
Example 2:
the embodiment provides a nano ferroferric oxide composite tea paper and a preparation method thereof, and the preparation method of the nano ferroferric oxide composite tea paper comprises the following steps:
s1: adding 200ml of sodium hydroxide solution with solute mass fraction of 1.9% into 5g of boiled and stemmed tea leaves, soaking for 12h, adding citric acid to adjust the pH value to 7, filtering, washing with water, and drying to obtain pretreated tea leaves;
s2: mixing the pretreated tea leaves obtained in the step S1 with water, a starch binder and cellulose fibers, adjusting the mixed solid content to 5%, and grinding to obtain slurry, wherein the mass ratio of the treated tea leaves to the water, the starch binder and the cellulose fibers is 1:50:0.06:0.2;
s3: pouring the slurry obtained in the step S2 into a paper liquid former, carrying out vacuum suction filtration to remove water, forming sheets, and drying at 80 ℃ to obtain a tea paper carrier;
s4: adding a silane coupling agent into a nano ferroferric oxide aqueous nano dispersion liquid with the mass fraction of 20% and the nano ferroferric oxide particle size of 30-50nm, controlling the mass fraction of the silane coupling agent in the dispersion liquid to be 0.5%, atomizing and spraying the silane coupling agent to the tea paper carrier obtained in the step S3, and freeze-drying the tea paper carrier at the temperature of-20 ℃ and under the environment of 6Pa to obtain the nano ferroferric oxide composite tea paper, wherein the pressure of compressed gas in the atomizing and spraying process is 30psi, and the silane coupling agent is A-171.
Through the inspection: the tea paper has a thickness of 0.8mm, a porosity of 75%, and a mass per unit area of 110g/m 2
Example 3:
the embodiment provides a nano ferroferric oxide composite tea paper and a preparation method thereof, and the preparation method of the nano ferroferric oxide composite tea paper comprises the following steps:
s1, adding 200ml of sodium hydroxide solution with solute mass fraction of 2.5% into 10g of boiled and stemmed tea leaves, soaking for 8 hours, adding citric acid to adjust the pH value to 7, filtering, washing with water, and drying to obtain pretreated tea leaves;
s2: mixing the pretreated tea leaves obtained in the step S1 with water, a starch binder and cellulose fibers, adjusting the mixed solid content to 3%, and grinding to obtain slurry, wherein the mass ratio of the treated tea leaves to the water, the starch binder and the cellulose fibers is 1:30:0.01:0.05;
s3: pouring the slurry obtained in the step S2 into a paper liquid former, carrying out vacuum suction filtration to remove water, carrying out sheet forming, and drying at 80 to 110 ℃ to obtain a tea paper carrier;
s4: adding a silane coupling agent into a nano ferroferric oxide aqueous nano dispersion liquid with the mass fraction of 20% and the nano ferroferric oxide particle size of 30-50nm, controlling the mass fraction of the silane coupling agent in the dispersion liquid to be 0.4%, atomizing and spraying the silane coupling agent to the tea paper carrier obtained in the step S3, and freeze-drying the tea paper carrier at the temperature of-10 ℃ and under the pressure of 4Pa to obtain the nano ferroferric oxide composite tea paper, wherein the pressure of compressed gas in the atomizing and spraying process is 30psi, and the silane coupling agent is FAS-13.
Through the inspection: the tea paper has a thickness of 1.0mm, a porosity of 88%, and a mass per unit area of 120g/m 2
Example 4
The embodiment provides a nano cobaltosic oxide composite tea paper and a preparation method thereof, and the preparation method of the nano cobaltosic oxide composite tea paper comprises the following steps:
s1: adding 200ml of sodium hydroxide solution with solute mass fraction of 2.0% into 8g of boiled and stemmed tea leaves, soaking for 10h, adding citric acid to adjust the pH value to 7, filtering, washing with water, and drying to obtain pretreated tea leaves;
s2: mixing the pretreated tea leaves obtained in the step S1 with water, a starch binder and cellulose fibers, adjusting the mixed solid content to 4%, and grinding to obtain slurry, wherein the mass ratio of the treated tea leaves to the water, the starch binder and the cellulose fibers is 1:40:0.06:0.1;
s3: pouring the slurry obtained in the step S2 into a paper liquid former, carrying out vacuum suction filtration to remove water, forming sheets, and drying at 100 ℃ to obtain a tea paper carrier;
s4: adding a silane coupling agent into a nano cobaltosic oxide aqueous nano dispersion liquid with the mass fraction of 20% and the nano cobaltosic oxide particle size of 30-50nm, controlling the mass fraction of the silane coupling agent in the dispersion liquid to be 0.3%, atomizing and spraying the silane coupling agent to the tea paper carrier obtained in the step S3, and freeze-drying the tea paper carrier at-15 ℃ and under the environment of 5Pa to obtain the nano cobaltosic oxide composite tea paper, wherein the pressure of compressed gas in the atomizing and spraying process is 30psi, and the silane coupling agent is KH-560.
Through the inspection: the tea paper has thickness of 1.1mm, porosity of 83%, and mass per unit area of 120g/m 2 。
Example 5:
the embodiment provides a nano cobaltosic oxide composite tea paper and a preparation method thereof, and the preparation method of the nano cobaltosic oxide composite tea paper comprises the following steps:
s1: adding 200ml of sodium hydroxide solution with solute mass fraction of 2.0% into 5g of boiled and stemmed tea leaves, soaking for 8h, adding citric acid to adjust the pH value to 7, filtering, washing with water, and drying to obtain pretreated tea leaves;
s2: mixing the pretreated tea leaves obtained in the step S1 with water, a starch binder and cellulose fibers, adjusting the mixed solid content to 5%, and grinding to obtain slurry, wherein the mass ratio of the treated tea leaves to the water, the starch binder and the cellulose fibers is 1:40:0.05:0.1;
s3: pouring the slurry obtained in the step S2 into a paper liquid former, carrying out vacuum suction filtration to remove water, carrying out sheet making and forming, and drying at 80-110 ℃ to obtain a tea paper carrier;
s4: adding a silane coupling agent into a nano cobaltosic oxide aqueous nano dispersion liquid with the mass fraction of 20% and the nano ferroferric oxide particle size of 30-50nm, controlling the mass fraction of the silane coupling agent in the dispersion liquid to be 0.4%, atomizing and spraying the silane coupling agent to the tea paper carrier obtained in the step S3, and freeze-drying the tea paper carrier at the temperature of-20 ℃ and under the environment of 4Pa to obtain the nano cobaltosic oxide composite tea paper, wherein the pressure of compressed gas in the atomizing and spraying process is 30psi, and the silane coupling agent is A-171.
And (4) checking: the tea paper has a thickness of 0.95mm, a porosity of 80%, and a mass per unit area of 110g/m 2
Example 6:
the embodiment provides a nano-cobaltosic oxide composite tea paper and a preparation method thereof, and the preparation method of the nano-ferroferric oxide composite tea paper comprises the following steps:
s1: adding 200ml of potassium hydroxide solution with solute mass fraction of 2.5% into 10g of boiled and stemmed tea leaves, soaking for 6 hours, adding citric acid to adjust the pH value to 7, filtering, washing with water, and drying to obtain pretreated tea leaves;
s2: mixing the pretreated tea leaves obtained in the step S1 with water, a starch binder and cellulose fibers, adjusting the mixed solid content to 3%, and grinding to obtain slurry, wherein the mass ratio of the treated tea leaves to the water, the starch binder and the cellulose fibers is 1:30:0.06:0.2;
s3: pouring the slurry into a paper liquid former, carrying out vacuum suction filtration to remove water, carrying out sheet forming, and drying at 90 ℃ to obtain a tea paper carrier;
s4: adding a silane coupling agent into a nano cobaltosic oxide aqueous nano dispersion liquid with the mass fraction of 20% and the nano cobaltosic oxide particle size of 30-50nm, controlling the mass fraction of the silane coupling agent in the dispersion liquid to be 0.5%, atomizing and spraying the silane coupling agent to the tea paper carrier obtained in the step S3, and freeze-drying the tea paper carrier at-10 ℃ and under the environment of 5Pa to obtain the nano cobaltosic oxide composite tea paper, wherein the pressure of compressed gas in the atomizing and spraying process is 30psi, and the silane coupling agent is FAS-13.
Through the inspection: the tea paper has a thickness of 0.8mm, a porosity of 80%, and a mass per unit area of 120g/m 2
Comparative example 1
The comparative example provides a nano ferroferric oxide composite tea paper and a preparation method thereof, and the preparation method of the nano ferroferric oxide composite tea paper comprises the following steps:
s1: adding 200ml of sodium hydroxide solution with solute mass fraction of 2.0% into 8g of boiled and stemmed tea leaves, soaking for 10h, adding citric acid to adjust the pH value to 7, filtering, washing with water, and drying to obtain pretreated tea leaves;
s2: mixing the pretreated tea leaves obtained in the step S1 with water, a starch binder and cellulose fibers, adjusting the mixed solid content to 4%, and grinding to obtain slurry, wherein the mass ratio of the treated tea leaves to the water, the starch binder and the cellulose fibers is 1:40:0.03:0.1;
s3: pouring the slurry obtained in the step S2 into a paper liquid former, carrying out vacuum suction filtration to remove water, forming sheets, and drying at 100 ℃ to obtain a tea paper carrier;
s4: adding a silane coupling agent into a nano ferroferric oxide aqueous nano dispersion liquid with the mass fraction of 20% and the nano ferroferric oxide particle size of 30-50nm, controlling the mass fraction of the silane coupling agent in the dispersion liquid to be 0.3%, soaking the tea paper carrier obtained in the step S3 in the nano ferroferric oxide added with the silane coupling agent for 12h, taking out and drying to obtain the nano ferroferric oxide composite tea paper, wherein the silane coupling agent is KH-560.
Through the inspection: the tea paper has a thickness of 0.6mm, a porosity of 90%, and a mass per unit area of 80g/m 2 。
Comparative example 2
The comparative example provides a nano ferroferric oxide composite tea paper and a preparation method thereof, and the preparation method of the nano ferroferric oxide composite tea paper comprises the following steps:
s1: adding 200ml of sodium hydroxide solution with solute mass fraction of 2.0% into 8g of boiled and stemmed tea leaves, soaking for 10 hours, adding citric acid to adjust the pH value to 7, filtering, washing with water, and drying to obtain pretreated tea leaves;
s2: mixing the pretreated tea leaves obtained in the step S1 with water, a starch binder and cellulose fibers, adjusting the mixed solid content to 4%, and grinding to obtain slurry, wherein the mass ratio of the treated tea leaves to the water, the starch binder and the cellulose fibers is 1:40:0.03:0.1;
s3: pouring the slurry obtained in the step S2 into a paper liquid former, carrying out vacuum suction filtration to remove water, carrying out sheet making and forming, and drying at 100 ℃ to obtain a tea paper carrier;
s4: and (3) atomizing and spraying the nano ferroferric oxide aqueous nano dispersion liquid with the mass fraction of 20% and the nano ferroferric oxide particle size of 30-50nm to the tea paper carrier obtained in the step (S3), and freeze-drying at-15 ℃ and under the environment of 5Pa to obtain the nano ferroferric oxide composite tea paper, wherein the pressure of compressed gas in the atomizing and spraying process is 30psi.
Through the inspection: the tea paper has a thickness of 0.7mm, a porosity of 87%, and a mass per unit area of 90g/m 2 。
Example of detection
(1) The nano magnetic oxide composite tea paper prepared in the examples 1 to 6 and the comparative examples 1 to 2 are respectively treated with heavy metal ion wastewater of the same source in equal amountAdsorbing heavy metal ions in the wastewater, wherein Pb in the heavy metal ions in the wastewater 2+ The initial mass concentration of (1) was 70mg/L and the amount of tea paper was 0.5g/L, and the adsorption equilibrium time and adsorption capacity were recorded by measuring at 25 ℃ and the results are shown in Table 1:
TABLE 1
Figure SMS_1
(2) The cycle capacity of the nano magnetic oxide composite tea paper prepared in the examples 1 to 6 and the comparative examples 1 to 2 is detected, and the test method comprises the following steps:
(1) the method comprises the following steps Soaking the nano magnetic oxide composite tea paper after adsorption balance in sufficient 1mol/L potassium carbonate solution for 30min, taking out, washing with water for 4 times to obtain recovered nano magnetic oxide composite tea paper, and reusing the recovered nano magnetic oxide composite tea paper for treating heavy metal ion wastewater with the same source and Pb in the heavy metal ion wastewater 2+ The initial mass concentration of (A) is 70mg/L, the dosage of the tea paper is 0.5g/L, the detection is carried out at 25 ℃, and the adsorption capacity at the adsorption equilibrium is recorded.
(2) The method comprises the following steps The results of statistics of adsorption capacity after repeating step (1) 7 times are shown in table 1.
TABLE 1
Figure SMS_2
(3) An optical photograph of the tea paper carrier prepared in example 1 is shown in fig. 1.
(4) An optical photograph of the nano-magnetic oxide composite tea paper prepared in example 1 is shown in fig. 2.
(5) The schematic diagram of the mechanical properties of the nano magnetic oxide composite tea paper prepared in the embodiment 1 is shown in fig. 3, and it can be seen from fig. 3 that the nano magnetic oxide composite tea paper prepared in the embodiment of the present invention can bear the gravity of a weight of 200g, and has a stable structure and outstanding mechanical properties.
(6) EXAMPLE 1 nanomagnetic preparedThe SEM image of the oxide composite tea paper is shown in FIG. 4, and the magnetic nano Fe can be seen from FIG. 4 3 O 4 Uniformly dispersed in the tea paper.
(7) The XRD pattern of the nano-magnetic oxide composite tea paper prepared in example 1 is shown in FIG. 5, and magnetic nano-Fe can be seen from FIG. 5 3 O 4 Successfully loaded in the tea paper.
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 or improvements made within the spirit and principle of the present invention should be included in the scope of the present invention.

Claims (6)

1. A preparation method of nanometer magnetic oxide composite tea paper for heavy metal ion adsorption is characterized by comprising the following steps:
s1: adding a sodium hydroxide solution with the mass fraction of 1.9-2.5% into the boiled and stemmed tea leaves, soaking, adding citric acid to adjust the pH value to 6-8, carrying out solid-liquid separation to obtain pretreated tea leaves, adding 20-40ml of the sodium hydroxide solution into each gram of tea leaves, and soaking for 6-12h;
s2: mixing the pretreated tea leaves with water, a starch binder and cellulose fibers according to a mass ratio of 1:30 to 50:0.01 to 0.06:0.05 to 0.2, adjusting the solid content of the mixed solution to 3 to 5 percent, and grinding to obtain slurry;
s3: removing water from the slurry, then sheet-making, forming and drying to obtain a tea paper carrier;
s4: adding an epoxy silane coupling agent into a nano magnetic oxide aqueous dispersion liquid with the mass fraction of 20-40%, controlling the mass fraction of the silane coupling agent in the nano magnetic oxide aqueous dispersion liquid to be 0.3-0.5%, atomizing and spraying the silane coupling agent to the tea paper carrier, and freeze-drying at the temperature of-20 to-10 ℃ and under the environment of 4 to 6Pa to obtain the nano magnetic oxide composite tea paper for adsorbing heavy metal ions.
2. The preparation method of the nano magnetic oxide composite tea paper for adsorbing heavy metal ions as claimed in claim 1, wherein the particle size of the nano magnetic oxide in the aqueous nano magnetic oxide dispersion is 30 to 50nm.
3. The preparation method of the nano magnetic oxide composite tea paper for adsorbing heavy metal ions according to claim 2, wherein the magnetic oxide is at least one of ferroferric oxide and cobaltosic oxide.
4. A nano magnetic oxide composite tea paper for heavy metal ion adsorption is characterized in that the nano magnetic oxide composite tea paper for heavy metal ion adsorption is prepared by the preparation method of the nano magnetic oxide composite tea paper for heavy metal ion adsorption according to any one of claims 1 to 3.
5. The nano magnetic oxide composite tea paper for adsorbing heavy metal ions as claimed in claim 4, wherein the thickness of the nano magnetic oxide composite tea paper is 0.8-1.2mm, the porosity is 70-90%, and the mass per unit area is 100-120g/m 2 。
6. The nano-magnetic oxide composite tea paper for adsorbing heavy metal ions as claimed in claim 5, wherein the particle size of the nano-magnetic oxide in the nano-magnetic oxide composite tea paper is 30 to 50nm.
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