CN111099667A - Organic silver and graphene composite circulating water treatment agent and use method thereof - Google Patents
Organic silver and graphene composite circulating water treatment agent and use method thereof Download PDFInfo
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- CN111099667A CN111099667A CN201811257494.6A CN201811257494A CN111099667A CN 111099667 A CN111099667 A CN 111099667A CN 201811257494 A CN201811257494 A CN 201811257494A CN 111099667 A CN111099667 A CN 111099667A
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
Abstract
The invention discloses an organic silver and graphene composite circulating water treatment agent and a using method thereof, and the organic silver and graphene composite circulating water treatment agent comprises the following components: the organic silver and graphene composite circulating water treatment agent comprises the following components in parts by weight: 40-50 parts of graphene oxide, 12-20 parts of acrylamide oligomer, 20-40 parts of mixed graphene oxide, 15-30 parts of organic silver and 20-30 parts of sodium bicarbonate, and the use method of the organic silver and graphene composite circulating water treatment agent comprises the following process steps: preparation of organic vehicle: the ratio of the organic solvent 2 to the organic solvent 1L is 1g, silver ion salt is dissolved in the organic solvent 2 to obtain silver ion salt solution, and the organic solvent 2 is the same as the organic solvent 1 used in the organic solvent 1). The method adopts the ultrasonically stripped graphene to avoid the defects introduced in the oxidation process, and the organic silver particles are uniformly compounded in the graphene layer in an electrophoretic deposition mode, so that the problem of agglomeration of the graphene is avoided.
Description
Technical Field
The invention relates to a preparation method of a water treatment agent, in particular to an organic silver and graphene composite circulating water treatment agent and a using method thereof.
Background
Since the discovery of graphene in 2004, the graphene has attracted extensive attention of researchers. The graphene has excellent mechanical, electronic, optical and thermal properties, and has great potential application value in the fields of microelectronics, energy storage, catalysis, biosensors and the like.
At present, the method for preparing the graphene/silver composite material mainly adopts a liquid-phase chemical reduction method, takes graphene oxide or reduced graphene as a raw material, adds a certain dispersant and silver ion salt to prepare a uniformly dispersed suspension, and then adds a reducing agent to reduce silver ions to be loaded on a graphene sheet layer. If graphene oxide is used as a raw material, the obtained composite material needs to be further reduced, and a large number of oxygen-containing groups on the surface of the graphene oxide are removed. However, the oxidized and stripped graphene still has the defect of more oxygen-containing groups after reduction, and various performances of the graphene are reduced.
Disclosure of Invention
The invention aims to provide an organic silver and graphene composite circulating water treatment agent, a using method and a manufacturing method thereof, and aims to solve the problems in the background technology.
The purpose of the invention is realized by the following technical scheme: an organic silver and graphene composite circulating water treatment agent comprises the following components and compositions: the organic silver and graphene composite circulating water treatment agent comprises the following components in parts by weight: 40-50 parts of graphene oxide, 12-20 parts of acrylamide oligomer, 20-40 parts of mixed graphene oxide, 15-30 parts of organic silver and 20-30 parts of sodium bicarbonate.
The use method of the organic silver and graphene composite circulating water treatment agent comprises the following process steps:
1) preparation of organic vehicle: dissolving silver ion salt in an organic solvent 2 at a ratio of 1g to 1L to obtain a silver ion salt solution, wherein the organic solvent 2 is the same as the organic solvent 1 used in the step 1); adding the obtained silver ion salt solution into the graphene dispersion liquid obtained in the step 1), enabling the concentration of silver ions to be 0.1-10mmol/L, controlling the temperature to be 20-40 ℃ and carrying out ultrasonic treatment at the power of 200W for 30min to enable graphene to adsorb the silver ions and carry positive charges, and obtaining the graphene dispersion liquid with the positive charges;
2) preparation of substrate silver paste: adding 30 g of the organic carrier solution prepared in the step 1) into a 200 ml beaker, keeping slowly stirring, sequentially measuring 2g of turpentine and 0.3 g of methyl silicone oil, adding the turpentine and the methyl silicone oil into the carrier solution, stirring at a high speed until the turpentine and the methyl silicone oil are uniformly mixed, then weighing 10 g of graphene micro-sheets, slowly adding the graphene micro-sheets, keeping stirring, after the addition is finished, stirring at a high speed until the graphene micro-sheets are uniformly dispersed in the carrier, measuring 60 g of silver-plated glass powder (the silver plating weight ratio is 40%), gradually and slowly adding the silver-plated glass powder, keeping stirring, and after the addition is finished, stirring at a high speed until the silver-plated glass powder is. The slurry is transferred to a three-roller machine for repeated rolling, dispersion and grinding until the fineness is below 5 mu m measured by a scraper blade fineness gauge, and finally about 100 g of base silver paste with uniformly dispersed particles is collected;
3) preparing a terminal silver paste: taking the graphene dispersion liquid with positive charges obtained in the step 2) as an electrolyte for electrophoretic deposition in an electrophoretic deposition pool; taking a metal conductive substrate such as copper, aluminum, nickel or stainless steel or a conductive substrate coated with metal or conductive materials such as copper, aluminum, nickel, stainless steel as a positive pole piece of the electrophoretic deposition pool; carrying out electrophoretic deposition by taking a conductive substrate without limiting the composition materials and the three-dimensional structure of the conductive substrate as a negative pole piece, namely depositing the graphene in the graphene dispersion liquid with positive charges on the negative pole piece; the conductive substrate without limiting the composition materials and the three-dimensional structure is a metal conductive matrix such as copper, aluminum, stainless steel and the like; or a conductive substrate coated with copper, aluminum, stainless steel or other metal or conductive material; or carbon fiber textiles such as carbon fiber paper, glassy carbon electrodes, conductive polymers such as polyaniline and other nonmetal conductive matrixes; and then, drying the cathode pole piece subjected to electrophoretic deposition in an oven at 80 ℃ for 12h to obtain a layer of graphene/silver composite material on the surface of the cathode pole piece.
The distance between the positive plate and the negative plate is controlled to be 1-50mm, preferably 5-10mm in the electrophoretic deposition process.
The applied voltage is 10-100V, preferably 40-60V.
The time is 1-60min, preferably 5-20 min.
The organic silver and graphene composite circulating water treatment agent comprises the following components in parts by weight: 40-50 parts of graphene oxide, 12-20 parts of acrylamide oligomer, 20-40 parts of mixed graphene oxide, 15-30 parts of organic silver and 20-30 parts of sodium bicarbonate.
The invention has the beneficial effects that: according to the organic silver and graphene composite circulating water treatment agent and the using method thereof, the final content and the microscopic morphology of the graphene and the silver simple substance can be controlled by adjusting the solid content of the graphene, the organic silver content and the experimental conditions in the deposition process. Furthermore, the defect caused in the oxidation process is avoided by the adoption of the graphene stripped by the ultrasonic wave in the preparation process, and the silver particles are uniformly compounded in the graphene layer in an electrophoretic deposition mode, so that the problem of agglomeration of the graphene is avoided. Has the advantages of simple process, easy production expansion, simple operation, etc.
Detailed Description
The following further description is provided in conjunction with the detailed description, but the detailed description below should not be construed as limiting the invention. Various modifications and variations obvious to those skilled in the art, which can be made on the basis of the present invention, should be within the scope of the present invention.
A use method of an organic silver and graphene composite circulating water treatment agent comprises the following process steps:
example 1:
1) preparation of organic vehicle: dissolving silver ion salt in an organic solvent 2 at a ratio of 1g to 1L to obtain a silver ion salt solution, wherein the organic solvent 2 is the same as the organic solvent 1 used in the step 1); adding the obtained silver ion salt solution into the graphene dispersion liquid obtained in the step 1), enabling the concentration of silver ions to be 0.1-10mmol/L, controlling the temperature to be 20-40 ℃ and carrying out ultrasonic treatment at the power of 200W for 30min to enable graphene to adsorb the silver ions and carry positive charges, and obtaining the graphene dispersion liquid with the positive charges;
2) preparation of substrate silver paste: adding 30 g of the organic carrier solution prepared in the step 1) into a 200 ml beaker, keeping slowly stirring, sequentially measuring 2g of turpentine and 0.3 g of methyl silicone oil, adding the turpentine and the methyl silicone oil into the carrier solution, stirring at a high speed until the turpentine and the methyl silicone oil are uniformly mixed, then weighing 10 g of graphene micro-sheets, slowly adding the graphene micro-sheets, keeping stirring, after the addition is finished, stirring at a high speed until the graphene micro-sheets are uniformly dispersed in the carrier, measuring 60 g of silver-plated glass powder (the silver plating weight ratio is 40%), gradually and slowly adding the silver-plated glass powder, keeping stirring, and after the addition is finished, stirring at a high speed until the silver-plated glass powder is. The slurry is transferred to a three-roller machine for repeated rolling, dispersion and grinding until the fineness is below 5 mu m measured by a scraper blade fineness gauge, and finally about 100 g of base silver paste with uniformly dispersed particles is collected;
3) preparing a terminal silver paste: taking the graphene dispersion liquid with positive charges obtained in the step 2) as an electrolyte for electrophoretic deposition in an electrophoretic deposition pool; taking a metal conductive substrate such as copper, aluminum, nickel or stainless steel or a conductive substrate coated with metal or conductive materials such as copper, aluminum, nickel, stainless steel as a positive pole piece of the electrophoretic deposition pool; carrying out electrophoretic deposition by taking a conductive substrate without limiting the composition materials and the three-dimensional structure of the conductive substrate as a negative pole piece, namely depositing the graphene in the graphene dispersion liquid with positive charges on the negative pole piece; the conductive substrate without limiting the composition materials and the three-dimensional structure is a metal conductive matrix such as copper, aluminum, stainless steel and the like; or a conductive substrate coated with copper, aluminum, stainless steel or other metal or conductive material; or carbon fiber textiles such as carbon fiber paper, glassy carbon electrodes, conductive polymers such as polyaniline and other nonmetal conductive matrixes; and then, drying the cathode pole piece subjected to electrophoretic deposition in an oven at 80 ℃ for 12h to obtain a layer of graphene/silver composite material on the surface of the cathode pole piece.
Example 2:
1) preparation of organic vehicle: dissolving silver ion salt in an organic solvent 2 at a ratio of 1.2g to 1L to obtain a silver ion salt solution, wherein the organic solvent 2 is the same as the organic solvent 1 used in the step (1); adding the obtained silver ion salt solution into the graphene dispersion liquid obtained in the step (1) to enable the concentration of silver ions to be 0.1-10mmol/L, controlling the temperature to be 10-20 ℃ and carrying out ultrasonic treatment at the power of 200W for 20min to enable graphene to adsorb the silver ions and carry positive charges, and obtaining the graphene dispersion liquid with the positive charges;
2) preparation of substrate silver paste: adding 30 g of the organic carrier solution prepared in the step 1) into a 200 ml beaker, keeping slowly stirring, sequentially measuring 2g of turpentine and 0.5 g of methyl silicone oil, adding the turpentine and the methyl silicone oil into the carrier solution, stirring at a high speed until the turpentine and the methyl silicone oil are uniformly mixed, then weighing 15 g of graphene micro-sheets, slowly adding the graphene micro-sheets, keeping stirring, after the addition is finished, stirring at a high speed until the graphene micro-sheets are uniformly dispersed in the carrier, measuring 60 g of silver-plated glass powder (the silver plating weight ratio is 40%), gradually and slowly adding the silver-plated glass powder, keeping stirring, and after the addition is finished, stirring at a high speed until the silver-plated glass powder is. The slurry is transferred to a three-roller machine for repeated rolling, dispersion and grinding until the fineness is below 5 mu m measured by a scraper blade fineness gauge, and finally about 100 g of base silver paste with uniformly dispersed particles is collected;
3) preparing a terminal silver paste: taking the graphene dispersion liquid with positive charges obtained in the step 2) as an electrolyte for electrophoretic deposition in an electrophoretic deposition pool; taking a metal conductive substrate such as copper, aluminum, nickel or stainless steel or a conductive substrate coated with metal or conductive materials such as copper, aluminum, nickel, stainless steel as a positive pole piece of the electrophoretic deposition pool; carrying out electrophoretic deposition by taking a conductive substrate without limiting the composition materials and the three-dimensional structure of the conductive substrate as a negative pole piece, namely depositing the graphene in the graphene dispersion liquid with positive charges on the negative pole piece; the conductive substrate without limiting the composition materials and the three-dimensional structure is a metal conductive matrix such as copper, aluminum, stainless steel and the like; or a conductive substrate coated with copper, aluminum, stainless steel or other metal or conductive material; or carbon fiber textiles such as carbon fiber paper, glassy carbon electrodes, conductive polymers such as polyaniline and other nonmetal conductive matrixes; and then, drying the cathode pole piece subjected to electrophoretic deposition in a 100 ℃ oven for 12h to obtain a layer of graphene/silver composite material on the surface of the cathode pole piece.
Example 3:
1) preparation of organic vehicle: dissolving silver ion salt in an organic solvent 2 at a ratio of 1.4g to 1L to obtain a silver ion salt solution, wherein the organic solvent 2 is the same as the organic solvent 1 used in the step (1); adding the obtained silver ion salt solution into the graphene dispersion liquid obtained in the step (1) to enable the concentration of silver ions to be 0.1-10mmol/L, controlling the temperature to be 20-30 ℃ and carrying out ultrasonic treatment with the power of 100W for 30min to enable graphene to adsorb the silver ions and carry positive charges, and obtaining the graphene dispersion liquid with the positive charges;
2) preparation of substrate silver paste: adding 30 g of the organic carrier solution prepared in the step 1) into a 200 ml beaker, keeping slowly stirring, sequentially measuring 2g of turpentine and 0.3 g of methyl silicone oil, adding the turpentine and the methyl silicone oil into the carrier solution, stirring at a high speed until the turpentine and the methyl silicone oil are uniformly mixed, then weighing 10 g of graphene micro-sheets, slowly adding the graphene micro-sheets, keeping stirring, after the addition is finished, stirring at a high speed until the graphene micro-sheets are uniformly dispersed in the carrier, measuring 60 g of silver-plated glass powder (the silver plating weight ratio is 40%), gradually and slowly adding the silver-plated glass powder, keeping stirring, and after the addition is finished, stirring at a high speed until the silver-plated glass powder is. The slurry is transferred to a three-roller machine for repeated rolling, dispersion and grinding until the fineness is below 5 mu m measured by a scraper blade fineness gauge, and finally about 100 g of base silver paste with uniformly dispersed particles is collected;
3) preparing a terminal silver paste: taking the graphene dispersion liquid with positive charges obtained in the step 2) as an electrolyte for electrophoretic deposition in an electrophoretic deposition pool; taking a metal conductive substrate such as copper, aluminum, nickel or stainless steel or a conductive substrate coated with metal or conductive materials such as copper, aluminum, nickel, stainless steel as a positive pole piece of the electrophoretic deposition pool; carrying out electrophoretic deposition by taking a conductive substrate without limiting the composition materials and the three-dimensional structure of the conductive substrate as a negative pole piece, namely depositing the graphene in the graphene dispersion liquid with positive charges on the negative pole piece; the conductive substrate without limiting the composition materials and the three-dimensional structure is a metal conductive matrix such as copper, aluminum, stainless steel and the like; or a conductive substrate coated with copper, aluminum, stainless steel or other metal or conductive material; or carbon fiber textiles such as carbon fiber paper, glassy carbon electrodes, conductive polymers such as polyaniline and other nonmetal conductive matrixes; and then, drying the cathode plate subjected to electrophoretic deposition in a 120 ℃ oven for 12h to obtain a layer of graphene/silver composite material on the surface of the cathode plate.
The above description is only a preferred embodiment of the application and is illustrative of the principles of the technology employed. It will be appreciated by a person skilled in the art that the scope of the invention as referred to in the present application is not limited to the embodiments with a specific combination of the above-mentioned features, but also covers other embodiments with any combination of the above-mentioned features or their equivalents without departing from the inventive concept. For example, the above features may be replaced with (but not limited to) features having similar functions disclosed in the present application.
Claims (5)
1. An organic silver and graphene composite circulating water treatment agent is characterized in that: it comprises the following components and compositions: the organic silver and graphene composite circulating water treatment agent comprises the following components in parts by weight: 40-50 parts of graphene oxide, 12-20 parts of acrylamide oligomer, 20-40 parts of mixed graphene oxide, 15-30 parts of organic silver and 20-30 parts of sodium bicarbonate.
2. The use method of the organic silver and graphene composite circulating water treatment agent according to claim 1, characterized by comprising the following steps: the method comprises the following process steps:
1) preparation of organic vehicle: dissolving silver ion salt in an organic solvent 2 at a ratio of 1g to 1L to obtain a silver ion salt solution, wherein the organic solvent 2 is the same as the organic solvent 1 used in the step 1); adding the obtained silver ion salt solution into the graphene dispersion liquid obtained in the step 1), enabling the concentration of silver ions to be 0.1-10mmol/L, controlling the temperature to be 20-40 ℃ and carrying out ultrasonic treatment at the power of 200W for 30min to enable graphene to adsorb the silver ions and carry positive charges, and obtaining the graphene dispersion liquid with the positive charges;
2) preparation of substrate silver paste: taking 30 g of the organic carrier solution prepared in the step 1), adding the organic carrier solution into a 200 ml beaker, keeping slow stirring, sequentially taking 2g of turpentine and 0.3 g of methyl silicone oil, adding the turpentine and the methyl silicone oil into the carrier solution, stirring at a high speed until the turpentine and the methyl silicone oil are uniformly mixed, then weighing 10 g of graphene micro-sheets, slowly adding the graphene micro-sheets, keeping stirring, after the addition is finished, stirring at a high speed until the graphene micro-sheets are uniformly dispersed in the carrier, then taking 60 g of silver-plated glass powder (the silver plating weight ratio is 40%), gradually and slowly adding the silver-plated glass powder, keeping stirring, and after the addition is finished, stirring at a high speed until the; the slurry is transferred to a three-roller machine for repeated rolling, dispersion and grinding until the fineness is below 5 mu m measured by a scraper blade fineness gauge, and finally about 100 g of base silver paste with uniformly dispersed particles is collected;
3) preparing a terminal silver paste: taking the graphene dispersion liquid with positive charges obtained in the step 2) as an electrolyte for electrophoretic deposition in an electrophoretic deposition pool; taking a metal conductive substrate such as copper, aluminum, nickel or stainless steel or a conductive substrate coated with metal or conductive materials such as copper, aluminum, nickel, stainless steel as a positive pole piece of the electrophoretic deposition pool; carrying out electrophoretic deposition by taking a conductive substrate without limiting the composition materials and the three-dimensional structure of the conductive substrate as a negative pole piece, namely depositing the graphene in the graphene dispersion liquid with positive charges on the negative pole piece; the conductive substrate without limiting the composition materials and the three-dimensional structure is a metal conductive matrix such as copper, aluminum, stainless steel and the like; or a conductive substrate coated with copper, aluminum, stainless steel or other metal or conductive material; or carbon fiber textiles such as carbon fiber paper, glassy carbon electrodes, conductive polymers such as polyaniline and other nonmetal conductive matrixes; and then, drying the cathode pole piece subjected to electrophoretic deposition in an oven at 80 ℃ for 12h to obtain a layer of graphene/silver composite material on the surface of the cathode pole piece.
3. The use method of the organic silver and graphene composite circulating water treatment agent according to claim 2, characterized by comprising the following steps: the distance between the positive plate and the negative plate is controlled to be 1-50mm, preferably 5-10mm in the electrophoretic deposition process.
4. The use method of the organic silver and graphene composite circulating water treatment agent according to claim 2, characterized by comprising the following steps: the applied voltage is 10-100V, preferably 40-60V.
5. The use method of the organic silver and graphene composite circulating water treatment agent according to claim 2, characterized by comprising the following steps: the time is 1-60min, preferably 5-20 min.
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Application publication date: 20200505 |