CN110004713B - Silver-containing graphene slurry, preparation method thereof and prepared product - Google Patents

Silver-containing graphene slurry, preparation method thereof and prepared product Download PDF

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CN110004713B
CN110004713B CN201910337500.7A CN201910337500A CN110004713B CN 110004713 B CN110004713 B CN 110004713B CN 201910337500 A CN201910337500 A CN 201910337500A CN 110004713 B CN110004713 B CN 110004713B
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parts
silver
containing graphene
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graphene
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CN110004713A (en
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商承杰
商蔚
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Beijing Jlsun High Tech Co ltd
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Beijing Jlsun High Tech Co ltd
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    • D—TEXTILES; PAPER
    • D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M11/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising
    • D06M11/73—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with carbon or compounds thereof
    • D06M11/74—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with carbon or compounds thereof with carbon or graphite; with carbides; with graphitic acids or their salts
    • D—TEXTILES; PAPER
    • D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M11/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising
    • D06M11/83—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with metals; with metal-generating compounds, e.g. metal carbonyls; Reduction of metal compounds on textiles
    • D—TEXTILES; PAPER
    • D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M13/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment
    • D06M13/10—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment with compounds containing oxygen
    • D06M13/224—Esters of carboxylic acids; Esters of carbonic acid
    • D06M13/2243—Mono-, di-, or triglycerides
    • D—TEXTILES; PAPER
    • D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M15/00—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment
    • D06M15/01—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment with natural macromolecular compounds or derivatives thereof
    • D06M15/03—Polysaccharides or derivatives thereof
    • D06M15/05—Cellulose or derivatives thereof
    • D06M15/09—Cellulose ethers
    • D—TEXTILES; PAPER
    • D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M15/00—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment
    • D06M15/19—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment with synthetic macromolecular compounds
    • D06M15/37—Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
    • D06M15/564—Polyureas, polyurethanes or other polymers having ureide or urethane links; Precondensation products forming them
    • D—TEXTILES; PAPER
    • D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M16/00—Biochemical treatment of fibres, threads, yarns, fabrics, or fibrous goods made from such materials, e.g. enzymatic
    • D—TEXTILES; PAPER
    • D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06P—DYEING OR PRINTING TEXTILES; DYEING LEATHER, FURS OR SOLID MACROMOLECULAR SUBSTANCES IN ANY FORM
    • D06P1/00—General processes of dyeing or printing textiles, or general processes of dyeing leather, furs, or solid macromolecular substances in any form, classified according to the dyes, pigments, or auxiliary substances employed
    • D06P1/44—General processes of dyeing or printing textiles, or general processes of dyeing leather, furs, or solid macromolecular substances in any form, classified according to the dyes, pigments, or auxiliary substances employed using insoluble pigments or auxiliary substances, e.g. binders
    • D06P1/46—General processes of dyeing or printing textiles, or general processes of dyeing leather, furs, or solid macromolecular substances in any form, classified according to the dyes, pigments, or auxiliary substances employed using insoluble pigments or auxiliary substances, e.g. binders using compositions containing natural macromolecular substances or derivatives thereof
    • D06P1/48—Derivatives of carbohydrates
    • D06P1/50—Derivatives of cellulose
    • D—TEXTILES; PAPER
    • D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06P—DYEING OR PRINTING TEXTILES; DYEING LEATHER, FURS OR SOLID MACROMOLECULAR SUBSTANCES IN ANY FORM
    • D06P1/00—General processes of dyeing or printing textiles, or general processes of dyeing leather, furs, or solid macromolecular substances in any form, classified according to the dyes, pigments, or auxiliary substances employed
    • D06P1/44—General processes of dyeing or printing textiles, or general processes of dyeing leather, furs, or solid macromolecular substances in any form, classified according to the dyes, pigments, or auxiliary substances employed using insoluble pigments or auxiliary substances, e.g. binders
    • D06P1/52—General processes of dyeing or printing textiles, or general processes of dyeing leather, furs, or solid macromolecular substances in any form, classified according to the dyes, pigments, or auxiliary substances employed using insoluble pigments or auxiliary substances, e.g. binders using compositions containing synthetic macromolecular substances
    • D06P1/5264—Macromolecular compounds obtained otherwise than by reactions involving only unsaturated carbon-to-carbon bonds
    • D06P1/5285—Polyurethanes; Polyurea; Polyguanides
    • D—TEXTILES; PAPER
    • D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06P—DYEING OR PRINTING TEXTILES; DYEING LEATHER, FURS OR SOLID MACROMOLECULAR SUBSTANCES IN ANY FORM
    • D06P1/00—General processes of dyeing or printing textiles, or general processes of dyeing leather, furs, or solid macromolecular substances in any form, classified according to the dyes, pigments, or auxiliary substances employed
    • D06P1/44—General processes of dyeing or printing textiles, or general processes of dyeing leather, furs, or solid macromolecular substances in any form, classified according to the dyes, pigments, or auxiliary substances employed using insoluble pigments or auxiliary substances, e.g. binders
    • D06P1/64—General processes of dyeing or printing textiles, or general processes of dyeing leather, furs, or solid macromolecular substances in any form, classified according to the dyes, pigments, or auxiliary substances employed using insoluble pigments or auxiliary substances, e.g. binders using compositions containing low-molecular-weight organic compounds without sulfate or sulfonate groups
    • D06P1/651—Compounds without nitrogen
    • D06P1/65106—Oxygen-containing compounds
    • D06P1/65125—Compounds containing ester groups

Abstract

The invention relates to the technical field of clothing processing, in particular to silver-containing graphene pulp, a preparation method thereof and a prepared product. The silver-containing graphene slurry comprises the following components in parts by weight: 0.2-10 parts of graphene, 0.1-15 parts of emulsifier, 10-80 parts of polar solvent, 1-10 parts of silver ammonia solution, 0.1-5 parts of reducing agent, 5-40 parts of adhesive and 0.2-8 parts of thickening agent. The silver-containing graphene paste prepared by the invention has excellent conductivity and antibacterial property, can greatly reduce bacteria on clothes, protect human health and eliminate static electricity, has the functions of heating by electrifying, emitting far infrared rays, resisting ultraviolet rays, insulating heat, keeping warm and the like, can be used for textile, leather and plastic products in printing, coating and other modes, and has wide application range.

Description

Silver-containing graphene slurry, preparation method thereof and prepared product
Technical Field
The invention belongs to the technical field of clothing processing, and particularly relates to silver-containing graphene pulp, a preparation method thereof and a prepared product.
Background
The printed fabric is a product with artistic quality, and the designed pattern is printed on the textile fabric by selecting dye or pigment, so that the pattern is formed on the fabric. The common printing process comprises three types of direct printing, dye-flooding printing and discharge printing. The direct printing is that the white or light color fabric is first printed with dye or pigment and then treated through steaming to obtain pattern. Dye-flooding printing is the printing of a substance on a fabric to drive the dye to dye or develop color, followed by dyeing or developing color to obtain a pattern on the dyed fabric. Discharge printing is a printing process in which a dyed fabric is printed with a substance that eliminates a dyeing dye to obtain a pattern on the dyed fabric.
The existing printing paste is an organic substance with general colloid property, can be dissolved or expanded in water to form sticky and plastic paste, can be used as a transfer agent for attaching dyes and other chemicals to fabrics, and is removed after printing and color fixing are finished. The size itself does not participate in the chemical reaction in printing and only acts as a mediator. Printing pastes can be divided into 6 categories according to their properties and attributes: starch and its derivatives, such as wheat starch, maize starch, flour and dextrin. ② vegetable gums, such as shellac, gum, seaweed gum and bletilla gum. ③ animal-based slurries, such as chitin gums. Mineral type slurries, such as white clay. Chemical pulp, such as hydroxymethyl cellulose, methyl cellulose, hydroxymethyl starch and emulsified pulp. Sixthly, other slurry, such as wood syrup, acorn powder, field kernel powder and the like.
However, the printing paste for the printed fabric prepared by the existing printing paste has poor antibacterial performance, cannot protect human health, and does not have the functions of far infrared heating, ultraviolet resistance, heat insulation, warmth retention and the like.
Disclosure of Invention
In order to solve the problems, the invention provides silver-containing graphene paste which comprises the following components in parts by weight: 0.2-10 parts of graphene, 0.1-15 parts of emulsifier, 10-80 parts of polar solvent, 1-10 parts of silver ammonia solution, 0.1-5 parts of reducing agent, 5-40 parts of adhesive and 0.2-8 parts of thickening agent.
As a preferable technical solution, the emulsifier is selected from one or more of polyoxyethylene ether, carboxymethyl cellulose, alkyl sulfonate, alkyl sulfate, glycerol stearate, glycerol cocoate, glycerol laurate, sorbitan oleate, sorbitan stearate, sorbitan trioleate, palmityl dimethyl tertiary amine, cocoyl dimethyl tertiary amine, and 1-methylpentanol.
As a preferable technical scheme, the silver-containing graphene paste further comprises 1-10 parts by weight of a conductive agent, wherein the conductive agent is conductive carbon black powder and/or conductive graphite powder.
As a preferred technical scheme, the polar solvent is selected from one or more of water, acetonitrile, dimethyl sulfoxide, methanol, ethanol, ethylene glycol, propylene glycol, glycerol and polyalcohol polymers.
As a preferred technical scheme, the reducing agent is selected from one or more of reducing sugar, formaldehyde, acetaldehyde and glutaraldehyde.
As a preferred technical scheme, the reducing sugar is selected from one or more of glucose, fructose, galactose, lactose and maltose.
As a preferable technical scheme, the adhesive is selected from one or more of polyvinyl alcohol, polyvinylpyrrolidone, gelatin, starch modifier, waterborne polyurethane and waterborne polyacrylate.
As a preferable technical scheme, the thickening agent is selected from one or more of methyl cellulose, hydroxypropyl methyl cellulose, hydroxyethyl cellulose, polyvinyl alcohol, polyvinylpyrrolidone and acrylic acid polymer.
The second aspect of the present invention provides a method for preparing silver-containing graphene paste, comprising the following steps:
s01: adding an emulsifier and a polar solvent into graphene, adding a silver ammonia solution after ultrasonic oscillation, uniformly stirring, and adding a silver reducing agent to obtain a mixture;
s02: and adding the mixture into a binder, a thickening agent and a conductive agent to obtain the silver-containing graphene slurry.
The third aspect of the invention provides an application of the silver-containing graphene pulp prepared by the preparation method in fabrics, non-woven fabrics, artificial leather, sponges, plastic films, flexible materials, clothes and bedding.
Has the advantages that: the silver-containing graphene paste prepared by the method has excellent conductivity and antibacterial property, can greatly reduce bacteria on clothes, protect human health and eliminate static electricity, has the functions of heating by electrifying, emitting far infrared rays, resisting ultraviolet rays, insulating heat, keeping warm and the like, can be used for textile, leather and plastic products in printing, coating and other modes, and has a wide application range.
Detailed Description
The technical features of the technical solutions provided by the present invention are further clearly and completely described below with reference to the specific embodiments, and the scope of protection is not limited thereto.
The words "preferred", "more preferred", and the like, in the present invention refer to embodiments of the invention that may provide certain benefits, under certain circumstances. However, other embodiments may be preferred, under the same or other circumstances. Furthermore, the recitation of one or more preferred embodiments does not imply that other embodiments are not useful, nor is it intended to exclude other embodiments from the scope of the invention.
In order to solve the problems, the invention provides silver-containing graphene paste which comprises the following components in parts by weight: 0.2-10 parts of graphene, 0.1-15 parts of emulsifier, 10-80 parts of polar solvent, 1-10 parts of silver ammonia solution, 0.1-5 parts of reducing agent, 5-40 parts of adhesive and 0.2-8 parts of thickening agent.
Graphene
The graphene is formed by sp from carbon atoms2The hybrid tracks form a hexagonal honeycomb lattice two-dimensional carbon nanomaterial.
In a preferred embodiment, the graphene of the present invention is graphene oxide; purchased from Hexagon, Sexiv materials science and technology, Inc. under model number SE 3122.
Emulsifier
The emulsifier of the present invention is a material capable of improving the surface tension between the various constituent phases in an emulsion to form a uniform and stable dispersion or emulsion. Emulsifiers are surface-active substances which have both hydrophilic and lipophilic groups in the molecule and which accumulate at the oil/water interface and reduce the interfacial tension and the energy required to form an emulsion, thereby increasing the energy of the emulsion.
In some embodiments, the emulsifier of the present invention is selected from one or more of polyoxyethylene ethers, carboxymethylcellulose, alkyl sulfonates, alkyl sulfates, glyceryl stearate, glyceryl cocoate, glyceryl laurate, sorbitan oleate, sorbitan stearate, sorbitan trioleate, palmityl dimethyl tertiary amine, cocoyl dimethyl tertiary amine, 1-methylpentanol.
In a preferred embodiment, the emulsifier of the present invention is glyceryl stearate.
Polar solvent
In some embodiments, the polar solvent of the present invention is selected from one or more of water, acetonitrile, dimethylsulfoxide, methanol, ethanol, ethylene glycol, propylene glycol, glycerol, polyol polymers.
In a preferred embodiment, the polar solvent of the present invention is a mixed solvent of water and ethanol, wherein the weight ratio of ethanol to water is 1: 5.
Silver ammonia solution
The silver-ammonia solution is silver nitrate ammonia water solution, also called vomit Lomb reagent, can oxidize aldehyde into carboxylic acid, and generates metal silver to deposit on the wall of a glass reactor vessel (silver mirror), and is commonly used for manufacturing glass liners and identifying reducing sugar.
In a preferred embodiment, the silver ammonia solution of the present invention is prepared by the following method: adding 100mL of 2% silver nitrate solution into a clean test tube, and then dropwise adding 2% dilute ammonia water while oscillating until the initially generated precipitate is just dissolved, thereby obtaining the silver-ammonia solution.
Reducing agent
The reducing agent of the invention is a substance which loses electrons or has electron deviation in oxidation-reduction reaction. The reducing agent itself has reducing properties and is oxidized, and the product is called an oxidation product. The reduction and the oxidation reaction are carried out simultaneously, that is, the reducing agent itself is oxidized to become an oxide while the reducing agent is oxidized with the reduced material. The reactant containing a certain substance with an increased valence is a reducing agent.
In some embodiments, the reducing agent of the present invention is selected from one or more of reducing sugars, formaldehyde, acetaldehyde, glutaraldehyde.
In a preferred embodiment, the reducing sugar of the present invention is selected from one or more of glucose, fructose, galactose, lactose, maltose.
In a more preferred embodiment, the reducing sugar of the present invention is glucose.
In a more preferred embodiment, the reducing agent of the present invention further comprises sodium maleate, sodium itaconate; more preferably, the reducing agent is a mixture of glucose, sodium maleate and sodium itaconate, and the weight ratio of the glucose, the sodium maleate and the sodium itaconate is 7 (0.5-1.2) to (0.5-1.2).
In the research process, the inventor finds that the nano silver on the graphene of the invention has uniform particle size and smooth surface, and the antibacterial effect of the product is excellent. The inventor conjectures that the sodium maleate and sodium itaconate contained in the reducing agent of the invention are helpful for reducing silver, and simultaneously carbon on the sodium maleate can form crystal growth, so that the grain size of the grown silver is in the range of 25-50nm, and the agglomeration condition is less. And when the weight ratio of the glucose to the sodium maleate to the sodium itaconate is 7 (0.5-1.2) to (0.5-1.2), the aggregation of the silver on the graphene is less, and the particle size is 25-50nm, and the inventor speculates that the itaconic acid has stronger chemical activity and can compete with the reduction reaction of the silver, so that the aggregation of the silver can be reduced.
Adhesive agent
The adhesive of the invention is a general name of various stress materials for connecting or jointing the same or different materials. There are three types, liquid, paste and solid.
In some embodiments, the binder of the present invention is selected from one or more of polyvinyl alcohol, polyvinyl pyrrolidone, gelatin, starch modification, aqueous polyurethane, aqueous polyacrylate.
In a preferred embodiment, the adhesive of the present invention is an aqueous polyurethane, available from Guangdong Yuebeautification industries, Inc.
Thickening agent
The thickening agent is a rheological aid, can thicken a product, and can endow the product with excellent mechanical properties and storage stability. An important class of adjuvants is for aqueous components of relatively low viscosity.
In some embodiments, the thickener of the present invention is selected from one or more of methylcellulose, hydroxypropyl methylcellulose, hydroxyethyl cellulose, polyvinyl alcohol, polyvinylpyrrolidone, acrylic acid polymers.
In a preferred embodiment, the thickener of the present invention is hydroxyethyl cellulose, available from Dalian Meilun Biotechnology Ltd.
In a preferred embodiment, the silver-containing graphene paste further comprises 1-10 parts of a conductive agent, wherein the conductive agent is conductive carbon black powder and/or conductive graphite powder.
Conductive agent
The conductive agent has the characteristics of small particle size, especially large specific surface area and excellent conductivity.
The conductive carbon black powder and the conductive graphite powder are not limited at all and can be any one purchased from the market, for example, the conductive carbon black powder in the embodiment of the invention is purchased from Tianjin Baichi chemical engineering and technology Co., Ltd, and the brand number is BC-90; the conductive graphite powder is purchased from Guangzhou large rubber raw materials Co.
The second aspect of the present invention provides a method for preparing silver-containing graphene paste, comprising the following steps:
s01: adding an emulsifier and a polar solvent into graphene, adding a silver ammonia solution after ultrasonic oscillation, uniformly stirring, and adding a silver reducing agent to obtain a mixture;
s02: and adding the mixture into a binder, a thickening agent and a conductive agent to obtain the silver-containing graphene slurry.
The third aspect of the invention provides an application of the silver-containing graphene pulp prepared by the preparation method in fabrics, non-woven fabrics, artificial leather, sponges, plastic films, flexible materials, clothes and bedding.
The present invention will now be described in detail by way of examples, and the starting materials used are commercially available unless otherwise specified.
Examples
Example 1
Embodiment 1 provides a silver-containing graphene paste, which comprises the following components in parts by weight: 0.2 part of graphene, 0.1 part of emulsifier, 10 parts of polar solvent, 1 part of silver ammonia solution, 0.1 part of reducing agent, 5 parts of adhesive, 0.2 part of thickening agent and 1 part of conductive agent.
The graphene is graphene oxide; purchased from Hexagon, Sexiv materials science and technology, Inc. under model number SE 3122.
The emulsifier is glyceryl stearate.
The polar solvent is a mixed solvent of water and ethanol, wherein the weight ratio of ethanol to water is 1: 5.
The silver ammonia solution is prepared by the following method: adding 100mL of 2% silver nitrate solution into a clean test tube, and then dropwise adding 2% dilute ammonia water while oscillating until the initially generated precipitate is just dissolved, thereby obtaining the silver-ammonia solution.
The reducing agent is a mixture of glucose, sodium maleate and sodium itaconate, and the weight ratio of the glucose to the sodium maleate to the sodium itaconate is 7:0.5: 1.2.
The adhesive is waterborne polyurethane and is purchased from Guangdong Yuebeautification industries, Inc.
The thickener is hydroxyethyl cellulose, purchased from Dalian Meiren Biotechnology Ltd.
The conductive agent is conductive carbon black powder which is purchased from Tianjin Baochi chemical technology Co., Ltd and is of a brand number BC-90.
A preparation method of silver-containing graphene slurry comprises the following steps:
s01: adding an emulsifier and a polar solvent into graphene, adding a silver ammonia solution after ultrasonic oscillation, uniformly stirring, and adding a silver reducing agent to obtain a mixture;
s02: and adding the mixture into a binder, a thickening agent and a conductive agent to obtain the silver-containing graphene slurry.
Example 2
Embodiment 2 provides a silver-containing graphene paste, which comprises the following components in parts by weight: 10 parts of graphene, 15 parts of emulsifier, 80 parts of polar solvent, 10 parts of silver ammonia solution, 5 parts of reducing agent, 40 parts of adhesive, 8 parts of thickening agent and 10 parts of conductive agent.
The graphene is graphene oxide; purchased from Hexagon, Sexiv materials science and technology, Inc. under model number SE 3122.
The emulsifier is glyceryl stearate.
The polar solvent is a mixed solvent of water and ethanol, wherein the weight ratio of ethanol to water is 1: 5.
The silver ammonia solution is prepared by the following method: adding 100mL of 2% silver nitrate solution into a clean test tube, and then dropwise adding 2% dilute ammonia water while oscillating until the initially generated precipitate is just dissolved, thereby obtaining the silver-ammonia solution.
The reducing agent is a mixture of glucose, sodium maleate and sodium itaconate, and the weight ratio of the glucose to the sodium maleate to the sodium itaconate is 7:1.2: 0.5.
The adhesive is waterborne polyurethane and is purchased from Guangdong Yuebeautification industries, Inc.
The thickener is hydroxyethyl cellulose, purchased from Dalian Meiren Biotechnology Ltd.
The conductive agent is conductive graphite powder, and is purchased from Guangzhou city big rubber raw material Co.
A method for preparing silver-containing graphene paste was the same as in example 1.
Example 3
Embodiment 3 provides a silver-containing graphene paste, which comprises the following components in parts by weight: 1 part of graphene, 1 part of emulsifier, 30 parts of polar solvent, 2 parts of silver ammonia solution, 0.5 part of reducing agent, 10 parts of adhesive, 2 parts of thickening agent and 2 parts of conductive agent.
The graphene is graphene oxide; purchased from Hexagon, Sexiv materials science and technology, Inc. under model number SE 3122.
The emulsifier is glyceryl stearate.
The polar solvent is a mixed solvent of water and ethanol, wherein the weight ratio of ethanol to water is 1: 5.
The silver ammonia solution is prepared by the following method: adding 100mL of 2% silver nitrate solution into a clean test tube, and then dropwise adding 2% dilute ammonia water while oscillating until the initially generated precipitate is just dissolved, thereby obtaining the silver-ammonia solution.
The reducing agent is a mixture of glucose, sodium maleate and sodium itaconate, and the weight ratio of the glucose to the sodium maleate to the sodium itaconate is 7:1: 0.5.
The adhesive is waterborne polyurethane and is purchased from Guangdong Yuebeautification industries, Inc.
The thickener is hydroxyethyl cellulose, purchased from Dalian Meiren Biotechnology Ltd.
The conductive agent is conductive carbon black powder which is purchased from Tianjin Baochi chemical technology Co., Ltd and is of a brand number BC-90.
A method for preparing silver-containing graphene paste was the same as in example 1.
Example 4
Embodiment 4 provides a silver-containing graphene paste, which comprises the following components in parts by weight: 3 parts of graphene, 5 parts of an emulsifier, 50 parts of a polar solvent, 5 parts of a silver ammonia solution, 3 parts of a reducing agent, 30 parts of an adhesive, 4 parts of a thickening agent and 5 parts of a conductive agent.
The graphene is graphene oxide; purchased from Hexagon, Sexiv materials science and technology, Inc. under model number SE 3122.
The emulsifier is glyceryl stearate.
The polar solvent is a mixed solvent of water and ethanol, wherein the weight ratio of ethanol to water is 1: 5.
The silver ammonia solution is prepared by the following method: adding 100mL of 2% silver nitrate solution into a clean test tube, and then dropwise adding 2% dilute ammonia water while oscillating until the initially generated precipitate is just dissolved, thereby obtaining the silver-ammonia solution.
The reducing agent is a mixture of glucose, sodium maleate and sodium itaconate, and the weight ratio of the glucose to the sodium maleate to the sodium itaconate is 7:1: 1.
The adhesive is waterborne polyurethane and is purchased from Guangdong Yuebeautification industries, Inc.
The thickener is hydroxyethyl cellulose, purchased from Dalian Meiren Biotechnology Ltd.
The conductive agent is conductive carbon black powder which is purchased from Tianjin Baochi chemical technology Co., Ltd and is of a brand number BC-90.
A method for preparing silver-containing graphene paste was the same as in example 1.
Example 5
Embodiment 5 provides a silver-containing graphene paste, which comprises the following components in parts by weight: 2 parts of graphene, 3 parts of an emulsifier, 40 parts of a polar solvent, 3.5 parts of a silver ammonia solution, 1 part of a reducing agent, 20 parts of an adhesive, 3 parts of a thickening agent and 4 parts of a conductive agent.
The graphene is graphene oxide; purchased from Hexagon, Sexiv materials science and technology, Inc. under model number SE 3122.
The emulsifier is glyceryl stearate.
The polar solvent is a mixed solvent of water and ethanol, wherein the weight ratio of ethanol to water is 1: 5.
The silver ammonia solution is prepared by the following method: adding 100mL of 2% silver nitrate solution into a clean test tube, and then dropwise adding 2% dilute ammonia water while oscillating until the initially generated precipitate is just dissolved, thereby obtaining the silver-ammonia solution.
The reducing agent is a mixture of glucose, sodium maleate and sodium itaconate, and the weight ratio of the glucose to the sodium maleate to the sodium itaconate is 7:1: 1.
The adhesive is waterborne polyurethane and is purchased from Guangdong Yuebeautification industries, Inc.
The thickener is hydroxyethyl cellulose, purchased from Dalian Meiren Biotechnology Ltd.
The conductive agent is conductive carbon black powder which is purchased from Tianjin Baochi chemical technology Co., Ltd and is of a brand number BC-90.
A method for preparing silver-containing graphene paste was the same as in example 1.
Example 6
Embodiment 6 provides a silver-containing graphene paste, which comprises the following components in parts by weight: 2 parts of graphene, 3 parts of an emulsifier, 40 parts of a polar solvent, 3.5 parts of a silver ammonia solution, 0.01 part of a reducing agent, 20 parts of an adhesive, 3 parts of a thickening agent and 4 parts of a conductive agent.
Example 6 differs from example 5 only in the parts by weight.
Example 7
Embodiment 7 provides a silver-containing graphene paste, which comprises the following components in parts by weight: 2 parts of graphene, 3 parts of an emulsifier, 40 parts of a polar solvent, 3.5 parts of a silver ammonia solution, 20 parts of a reducing agent, 20 parts of an adhesive, 3 parts of a thickening agent and 4 parts of a conductive agent.
Example 7 differs from example 5 only in the parts by weight.
Example 8
Embodiment 8 provides a silver-containing graphene paste, which comprises the following components in parts by weight: 2 parts of graphene, 3 parts of an emulsifier, 40 parts of a polar solvent, 3.5 parts of a silver ammonia solution, 1 part of a reducing agent, 20 parts of an adhesive, 3 parts of a thickening agent and 4 parts of a conductive agent.
Example 8 differs from example 5 in that: the reducing agent is a mixture of glucose, sodium maleate and sodium itaconate, and the weight ratio of the glucose to the sodium maleate to the sodium itaconate is 7:0.01: 1.
Example 9
Embodiment 9 provides a silver-containing graphene paste, which comprises the following components in parts by weight: 2 parts of graphene, 3 parts of an emulsifier, 40 parts of a polar solvent, 3.5 parts of a silver ammonia solution, 1 part of a reducing agent, 20 parts of an adhesive, 3 parts of a thickening agent and 4 parts of a conductive agent.
Example 9 differs from example 5 in that: the reducing agent is a mixture of glucose, sodium maleate and sodium itaconate, and the weight ratio of the glucose to the sodium maleate to the sodium itaconate is 7:10: 1.
Example 10
Embodiment 10 provides a silver-containing graphene paste, which comprises the following components in parts by weight: 2 parts of graphene, 3 parts of an emulsifier, 40 parts of a polar solvent, 3.5 parts of a silver ammonia solution, 1 part of a reducing agent, 20 parts of an adhesive, 3 parts of a thickening agent and 4 parts of a conductive agent.
Example 10 differs from example 5 in that: the reducing agent is a mixture of glucose, sodium maleate and sodium itaconate, and the weight ratio of the glucose to the sodium maleate to the sodium itaconate is 7:1: 0.01.
Example 11
Embodiment 11 provides a silver-containing graphene paste, comprising the following components in parts by weight: 2 parts of graphene, 3 parts of an emulsifier, 40 parts of a polar solvent, 3.5 parts of a silver ammonia solution, 1 part of a reducing agent, 20 parts of an adhesive, 3 parts of a thickening agent and 4 parts of a conductive agent.
Example 11 differs from example 5 in that: the reducing agent is a mixture of glucose, sodium maleate and sodium itaconate, and the weight ratio of the glucose to the sodium maleate to the sodium itaconate is 7:1: 10.
Evaluation of Performance
And (3) testing antibacterial performance: the test was performed according to AATCC 100-.
And (3) testing the particle size of the nano silver: and (4) adopting a scanning electron microscope for characterization, and testing the particle size of the nano silver of the silver-containing graphene slurry.
TABLE 1
Figure BDA0002039636830000101

Claims (8)

1. The silver-containing graphene slurry is characterized by comprising the following components in parts by weight: 0.2-10 parts of graphene, 0.1-15 parts of emulsifier, 10-80 parts of polar solvent, 1-10 parts of silver ammonia solution, 0.1-5 parts of reducing agent, 5-40 parts of adhesive and 0.2-8 parts of thickening agent; the reducing agent is a mixture of glucose, sodium maleate and sodium itaconate, and the weight ratio of the glucose to the sodium maleate to the sodium itaconate is 7 (0.5-1.2) to 0.5-1.2.
2. The silver-containing graphene paste according to claim 1, wherein the emulsifier is selected from one or more of polyoxyethylene ethers, carboxymethylcellulose, alkyl sulfonates, alkyl sulfates, glyceryl stearate, glyceryl cocoate, glyceryl laurate, sorbitan oleate, sorbitan stearate, sorbitan trioleate, palmityl dimethyl tertiary amine, cocoyl dimethyl tertiary amine, 1-methylpentanol.
3. The silver-containing graphene paste according to claim 1, further comprising 1-10 parts by weight of a conductive agent, wherein the conductive agent is conductive carbon black powder and/or conductive graphite powder.
4. The silver-containing graphene paste according to claim 1, wherein the polar solvent is selected from one or more of water, acetonitrile, dimethyl sulfoxide, methanol, ethanol, ethylene glycol, propylene glycol, glycerol, and polyol polymers.
5. The silver-containing graphene paste according to claim 1, wherein the binder is selected from one or more of polyvinyl alcohol, polyvinylpyrrolidone, gelatin, starch modifier, aqueous polyurethane, and aqueous polyacrylate.
6. The silver-containing graphene paste according to claim 1, wherein the thickener is one or more selected from the group consisting of methylcellulose, hydroxypropyl methylcellulose, hydroxyethyl cellulose, polyvinyl alcohol, polyvinyl pyrrolidone, and acrylic acid polymer.
7. The method for preparing the silver-containing graphene paste according to claim 3, comprising the following steps:
s01: adding an emulsifier and a polar solvent into graphene, adding a silver ammonia solution after ultrasonic oscillation, uniformly stirring, and adding a silver reducing agent to obtain a mixture;
s02: and adding the mixture into a binder, a thickening agent and a conductive agent to obtain the silver-containing graphene slurry.
8. The use of the silver-containing graphene paste prepared according to the preparation method of claim 7 in fabrics, non-woven fabrics, artificial leathers, sponges, plastic films, clothing, bedding.
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