CN114774183B - Zinc borate/Fe-BDC nano composite lubricating oil additive and preparation method thereof - Google Patents
Zinc borate/Fe-BDC nano composite lubricating oil additive and preparation method thereof Download PDFInfo
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- CN114774183B CN114774183B CN202210505724.6A CN202210505724A CN114774183B CN 114774183 B CN114774183 B CN 114774183B CN 202210505724 A CN202210505724 A CN 202210505724A CN 114774183 B CN114774183 B CN 114774183B
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- C10M161/00—Lubricating compositions characterised by the additive being a mixture of a macromolecular compound and a non-macromolecular compound, each of these compounds being essential
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- C10M177/00—Special methods of preparation of lubricating compositions; Chemical modification by after-treatment of components or of the whole of a lubricating composition, not covered by other classes
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- C10M2201/00—Inorganic compounds or elements as ingredients in lubricant compositions
- C10M2201/087—Boron oxides, acids or salts
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- C10M2209/00—Organic macromolecular compounds containing oxygen as ingredients in lubricant compositions
- C10M2209/10—Macromolecular compoundss obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10N—INDEXING SCHEME ASSOCIATED WITH SUBCLASS C10M RELATING TO LUBRICATING COMPOSITIONS
- C10N2030/00—Specified physical or chemical properties which is improved by the additive characterising the lubricating composition, e.g. multifunctional additives
- C10N2030/06—Oiliness; Film-strength; Anti-wear; Resistance to extreme pressure
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- 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
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/10—Process efficiency
Abstract
The invention discloses a preparation method of zinc borate/Fe-BDC nano composite lubricating oil additive, the lubricating oil additive prepared by the invention has excellent friction performance and dispersion performance, strong oxidation resistance and high viscosity, and the invention selects boric acid and zinc nitrate to synthesize zinc borate particles and MOF synthetic liquid to mix, so that the zinc borate particles are loaded on the surface of MOF to the greatest extent, and the functions of the zinc borate particles and the MOF synthetic liquid are fully exerted; meanwhile, the invention selects the microwave synthesis method, which is simple, convenient and rapid, can reduce the reaction time and simplify the reaction flow.
Description
Technical Field
The invention belongs to the technical field of preparation of lubricating materials, and particularly relates to a zinc borate/Fe-BDC nano composite lubricating oil additive and a preparation method thereof.
Background
In recent years, the continuous development of industrialization causes the aggravation of mechanical friction and abrasion phenomena, and the conventional nano additives containing sulfur, phosphorus, chlorine and other elements cannot meet the requirements of the modern society. Therefore, metal Organic Frameworks (MOFs) have been increasingly attracting attention of many researchers as a novel green lubricating oil additive which is highly effective and environmentally friendly and has good dispersibility. As an organic-inorganic hybrid material, 2D metal-organic frameworks (2D MOFs) have designable organic ligands that can effectively enhance their compatibility with lubricating oils, producing good interfacial interactions with lubricant surfaces. However, the tribological properties of the single MOF in lubricating oil are easily affected by the structure, and defects easily occur in the friction process, so that the friction performance of the single MOF cannot be well exerted. The tribological properties of MOFs have also been demonstrated to be effective by combining MOFs with other friction agents having antiwear and antifriction properties into composites.
The borate lubricating oil additive is used as a high-efficiency nontoxic traditional environment-friendly inorganic nano additive, and can lead borate to move directionally by virtue of attraction formed by electron orbit cavities around boron atoms and deposit on a friction pair to play a role in extreme pressure wear resistance. The borate-based composite material has high adsorption performance and excellent self-lubricating property, so that the borate-based composite material has wide application prospect as a lubricating oil additive, and particularly has wide application prospect in a plurality of severe environments. In the past studies, borates have been prepared into composite lubricating materials by using a heterogeneous coprecipitation method, a hydrothermal method, an in-situ synthesis method, and the like, and also exhibit excellent lubricating properties. .
Disclosure of Invention
This section is intended to outline some aspects of embodiments of the invention and to briefly introduce some preferred embodiments. Some simplifications or omissions may be made in this section as well as in the description summary and in the title of the application, to avoid obscuring the purpose of this section, the description summary and the title of the invention, which should not be used to limit the scope of the invention.
The present invention has been made in view of the above and/or problems occurring in the prior art.
Therefore, the invention aims to overcome the defects in the prior art and provide a preparation method of the zinc borate/Fe-BDC nano composite lubricating oil additive.
In order to solve the technical problems, the invention provides the following technical scheme:
iron sulfate FeSO 4 ·7H 2 O and 1,3, 5-benzene tricarboxylic acid are dissolved in N, N-dimethylformamide, and stirred until the O and the 1,3, 5-benzene tricarboxylic acid are completely dissolved, so as to obtain a mixed solution A;
and respectively dissolving borax and zinc nitrate in deionized water, and stirring to form borax solution and zinc nitrate solution.
Mixing and stirring the two solutions to form milky turbid liquid, and carrying out suction filtration and drying to obtain zinc borate nano particles;
zinc borate particles are dispersed in deionized water to form uniformly dispersed zinc borate solution;
adding zinc borate solution into the mixed solution A, stirring and then carrying out ultrasonic treatment until the zinc borate is completely dispersed, and placing the solution into a microwave oven for microwave synthesis after the solution is completely dispersed;
and (3) after synthesis, carrying out suction filtration, washing and drying to obtain the zinc borate/Fe-BDC nano composite lubricating material.
As a preferred embodiment of the present invention, wherein: the ferric sulfate FeSO 4 ·7H 2 The addition amount of O is 0.834 g-1.668 g, the addition amount of 1,3, 5-benzene tricarboxylic acid is 0.420 g-0.840 g, and the amount of N, N-dimethylformamide60ml.
As a preferred embodiment of the present invention, wherein: the stirring is carried out to form borax solution and zinc nitrate solution, wherein the adding proportion of borax to zinc nitrate is 1:1 to 1.5g, the addition amount is respectively 10 to 15g, and the amount of deionized water is 100ml.
As a preferred embodiment of the present invention, wherein: and stirring to form borax solution and zinc nitrate solution, wherein the stirring temperature is 50-80 ℃ and the stirring time is 3-6h.
As a preferred embodiment of the present invention, wherein: the two solutions are mixed and stirred to form milky turbid liquid, wherein the stirring temperature is room temperature, and the stirring time is 30-60min.
As a preferred embodiment of the present invention, wherein: the zinc borate particles are dispersed in deionized water, and the addition amount of the particles is 5g-10g.
As a preferred embodiment of the present invention, wherein: and adding the zinc borate solution into the mixed solution A in a dropwise adding mode, wherein the dropwise adding frequency is 1-3 drops/min.
As a preferred embodiment of the present invention, wherein: the stirring is carried out before the ultrasonic treatment, wherein the ultrasonic power is 300-400W, and the time is 15-30 min.
As a preferred embodiment of the present invention, wherein: the microwave hydrothermal synthesis is carried out, the microwave frequency is set to be 2.45GHz, the power is 300W, and the time is 3-5min.
It is still another object of the present invention to overcome the deficiencies of the prior art and to provide a product made by the method of preparing zinc borate/Fe-BDC nanocomposite lubricating oil additives.
The invention has the beneficial effects that:
(1) The invention adopts a microwave synthesis method, and the method is quick, convenient and efficient, and can generate larger heat and pressure in a short period of minutes so as to quickly synthesize the compound; meanwhile, the prepared composite material has a nano-scale and micro-scale structure, is easy to enter a friction pair contact area in a friction process, has high zinc borate element content in surface compounding, and can effectively play a role in synergistic lubrication.
(2) The traditional zinc borate nano particles are easy to agglomerate in lubricating oil, and the MOF serving as a lubricant has some defects, and the invention combines the advantages of the zinc borate nano particles and the MOF to complement and synergistically, so that the zinc borate nano particles can play a good synergistic lubrication role in interlayer sliding and rolling effect of particles in base oil, and the final antifriction and antiwear properties are greatly improved compared with those of pure base oil.
(3) The nano lubrication composite material of zinc borate/Fe-BDC prepared by the invention has a unique on-chip load ball particle structure, and zinc borate nano particles show smaller nano particles, and are different from pure zinc borate or Fe-BDC in morphology, and the material with the shape can play a role of interlayer sliding in the friction process, so that the friction coefficient is reduced.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the drawings that are needed in the description of the embodiments will be briefly described below, it being obvious that the drawings in the following description are only some embodiments of the present invention, and that other drawings may be obtained according to these drawings without inventive effort for a person skilled in the art. Wherein:
FIG. 1 is an SEM photograph of a zinc borate/Fe-BDC composite prepared in example 1 of the present invention;
FIG. 2 is a diagram showing the zinc borate/Fe-BDC prepared in the practice of the present invention 1.
The method for measuring the wear resistance and antifriction performance comprises the following steps: the friction experiment is carried out at room temperature by adopting a four-ball friction tester, the prepared nano composite lubricating material is used as an additive to be applied to base oil, and the additive amount of the composite material is 0.04wt%;
the method for measuring the dispersion performance in the invention comprises the following steps: dispersing the compound in the base oil according to 0.04wt%, standing for two weeks, and measuring the Uv-vis curve of the compound, and comparing the Uv-vis curve with the initial curve to obtain a dispersion stability stable value;
the kinematic viscosity in the invention is measured by a glass capillary viscometer;
the oxidation resistance in the invention is measured by a differential scanning calorimeter;
the raw materials used in the invention are as follows: iron sulfate heptahydrate (FeSO4.7H2O, > 99.0%), 1,3, 5-benzenetricarboxylic acid (H3 BTC), N-N dimethylformamide (DMF, > 99.5%), borax (Na2B4O7.10H2O, > 99.0%), and zinc nitrate (Zn (NO 3) 2.6H2O > 99.0%) were all purchased from national pharmaceutical and chemical reagent Co.
The device used in the invention comprises:
magnetic stirrer: model HJ-4A of Hezhou national electrical Co., ltd;
analytical balance: sidoriscom instruments (Beijing);
suction filtration circulating water vacuum pump: nanjing Col instruments, inc., model: SHZ-III;
electric heating constant temperature drying cabinet: shanghai precision macro laboratory equipment Co., ltd;
four-ball friction tester (MMW-1,Jinan ChendaLtd Co, jinan City, china);
cary 5000 Spectrophotometer (Varian, USA).
Detailed Description
In order that the above-recited objects, features and advantages of the present invention will become more apparent, a more particular description of the invention will be rendered by reference to specific embodiments thereof which are illustrated in the appended drawings.
In the following description, numerous specific details are set forth in order to provide a thorough understanding of the present invention, but the present invention may be practiced in other ways other than those described herein, and persons skilled in the art will readily appreciate that the present invention is not limited to the specific embodiments disclosed below.
Further, reference herein to "one embodiment" or "an embodiment" means that a particular feature, structure, or characteristic can be included in at least one implementation of the invention. The appearances of the phrase "in one embodiment" in various places in the specification are not necessarily all referring to the same embodiment, nor are separate or alternative embodiments mutually exclusive of other embodiments.
Example 1
Will be 0.834g FeSO 4 ·7H 2 O and 0.420g of 1,3, 5-benzene tricarboxylic acid are dissolved in 60ml of N, N-dimethylformamide, and stirred until complete dissolution;
10g of borax and 13g of zinc nitrate were dissolved in deionized water, respectively, and stirred to form borax solution and zinc nitrate solution. Mixing and stirring the two solutions at 60 ℃ for 3 hours to form milky turbid liquid, and drying after suction filtration to synthesize zinc borate nano particles;
5g of zinc borate particles were dispersed in 10ml of deionized water to form a uniformly dispersed solution.
The zinc borate solution was added dropwise to the mixed solution A at a frequency of 2 drops/min, and after stirring, the solution was sonicated at a power of 350W for 20min until the zinc borate was completely dispersed.
After the solution is completely dispersed, placing the solution in a microwave oven for microwave hydrothermal synthesis for 4 minutes, wherein the microwave frequency is set to be 2.45GHz, and the power is set to be 300W;
and (3) carrying out suction filtration, washing and drying on the solution to obtain a composite product.
The size of the zinc borate/Fe-BDC nano composite lubricating oil material prepared by the method is 600nm, and the content of the contained composite B element and Zn element respectively reaches 31.28at.% and 6.15at.%; when the additive is applied to base oil, the friction coefficient and the abrasion mark diameter are respectively reduced by 72.5 percent and 52.15 percent, and the dispersion stability value is 70.1.
Example 2
Adjusting the adding proportion of borax and zinc nitrate to be 1:1,1:1.1,1:1.2,1:1.4,1:1.5, the remainder of the procedure is the same as in example 1.
Table 1 shows the properties of the zinc borate/Fe-BDC nanocomposite lubricant prepared in example 2
TABLE 1
As can be seen from table 1, zinc borate particles are too small to be agglomerated together, and cannot be loaded on the surface of the MOF, and the loading amount of the zinc borate particles on the surface of the MOF is relatively small when the zinc borate particles are too large, according to the invention, the method comprises the following steps of: 1.3, the zinc borate particles synthesized according to the proportion have moderate particle size, and can be loaded on the surface of the MOF to the greatest extent.
Example 3
The procedure of example 1 was repeated except that the amounts of zinc borate particles added were adjusted to 3g, 4g, 6g, 7g, 8g, 9g, 10g and 11g, respectively.
Table 2 shows the properties of the zinc borate/Fe-BDC nanocomposite lubricant prepared in example 3 and its antiwear properties in a base oil.
TABLE 2
As can be seen from table 2, when zinc borate particles are excessively added, the zinc borate particles are unevenly dispersed, and are easily agglomerated together in the compounding process, so that the particles are too large to be compounded with MOF; too few particles incorporated on the MOF surface will reduce resulting in poor performance.
Example 4
Will be 0.834g FeSO 4 ·7H 2 O and 0.420g of 1,3, 5-benzene tricarboxylic acid are dissolved in 60ml of N, N-dimethylformamide, and stirred until complete dissolution;
10g of borax and 13g of zinc nitrate were dissolved in deionized water, respectively, and stirred to form borax solution and zinc nitrate solution. Mixing and stirring the two solutions at 60 ℃ for 3 hours to form milky turbid liquid, and drying after suction filtration to synthesize zinc borate nano particles;
5g of zinc borate particles were dispersed in 10ml of deionized water to form a uniformly dispersed solution.
The zinc borate solution is directly mixed with the mixed solution A, and is stirred and then is subjected to ultrasonic treatment with power of 350W for 20min until the zinc borate is completely dispersed.
After the solution is completely dispersed, placing the solution in a microwave oven for microwave hydrothermal synthesis for 4 minutes, wherein the microwave frequency is set to be 2.45GHz, and the power is set to be 300W;
and (3) carrying out suction filtration, washing and drying on the solution to obtain a composite product.
Example 5
Will be 0.834g FeSO 4 ·7H 2 O and 0.420g of 1,3, 5-benzene tricarboxylic acid are dissolved in 60ml of N, N-dimethylformamide, and stirred until complete dissolution;
10g of borax and 13g of zinc nitrate were dissolved in deionized water, respectively, and stirred to form borax solution and zinc nitrate solution. Mixing and stirring the two solutions at 60 ℃ for 3 hours to form milky turbid liquid, and drying after suction filtration to synthesize zinc borate nano particles;
5g of zinc borate particles were dispersed in 10ml of deionized water to form a uniformly dispersed solution.
The zinc borate solution was added dropwise to the mixed solution A at a rate of 5 drops/min, and after stirring, the solution was sonicated at a power of 350W for 20min until the zinc borate was completely dispersed.
After the solution is completely dispersed, placing the solution in a microwave oven for microwave hydrothermal synthesis for 4 minutes, wherein the microwave frequency is set to be 2.45GHz, and the power is set to be 300W;
and (3) carrying out suction filtration, washing and drying on the solution to obtain a composite product.
Example 6
Will be 0.834g FeSO 4 ·7H 2 O and 0.420g of 1,3, 5-benzene tricarboxylic acid are dissolved in 60ml of N, N-dimethylformamide, and stirred until complete dissolution;
10g of borax and 13g of calcium chloride are respectively dissolved in deionized water, and are stirred to form borax solution and calcium chloride solution. Mixing and stirring the two solutions at 60 ℃ for 3 hours to form milky turbid liquid, and drying after suction filtration to synthesize calcium borate nano particles;
5g of calcium borate particles were dispersed in 10ml of deionized water to form a uniformly dispersed solution.
The calcium borate solution was added dropwise to the mixed solution A at a rate of 2 drops/min, and after stirring, the solution was sonicated at a power of 350W for 20min until the calcium borate was completely dispersed.
After the solution is completely dispersed, placing the solution in a microwave oven for microwave hydrothermal synthesis for 4 minutes, wherein the microwave frequency is set to be 2.45GHz, and the power is set to be 300W;
and (3) carrying out suction filtration, washing and drying on the solution to obtain a composite product.
Example 7
Will be 0.834g FeSO 4 ·7H 2 O and 0.420g of 1,3, 5-benzene tricarboxylic acid are dissolved in 60ml of N, N-dimethylformamide, and stirred until complete dissolution;
respectively dissolving 10g of borax and 13g of zinc nitrate in deionized water, and stirring to form borax solution and zinc nitrate solution;
directly mixing the two solutions with the mixed solution A, stirring, and performing ultrasonic treatment with power of 350W for 20min; placing the mixture in a microwave oven for microwave hydrothermal treatment for 4 minutes to synthesize, wherein the microwave frequency is set to be 2.45GHz, and the power is set to be 300W;
and (3) carrying out suction filtration, washing and drying on the solution to obtain a composite product.
Example 8
Will be 0.834g FeSO 4 ·7H 2 O and 0.420g of 1,3, 5-benzene tricarboxylic acid are dissolved in 60ml of N, N-dimethylformamide, and stirred until complete dissolution;
10g of borax and 13g of zinc nitrate were dissolved in deionized water, respectively, and stirred to form borax solution and zinc nitrate solution. Mixing and stirring the two solutions at 60 ℃ for 3 hours to form milky turbid liquid, and drying after suction filtration to synthesize zinc borate nano particles;
5g of zinc borate particles were dispersed in 10ml of deionized water to form a uniformly dispersed solution.
The zinc borate solution was added dropwise to the mixed solution A at a frequency of 2 drops/min, and after stirring, the solution was sonicated at a power of 350W for 20min until the zinc borate was completely dispersed.
After the solution is completely dispersed, placing the solution in a homogeneous reactor, and keeping the solution at 160 ℃ for 12 hours for in-situ hydrothermal synthesis;
and (3) carrying out suction filtration, washing and drying on the solution to obtain a composite product.
Table 3 shows the properties of the zinc borate/Fe-BDC nanocomposite lubricating materials prepared in examples 4 to 8, their antiwear and antifriction properties in base oils, and their dispersion properties, oxidation resistance properties, and viscosity.
TABLE 3 Table 3
It can be seen from table 3 that the oxidation resistance and viscosity at 100 ℃ of the composite lubricating material prepared by the invention are obviously higher than those of example 6, because the binding force of the B-O bond in the zinc borate structure combined by zinc and boric acid is strong, the formed crystal is stable and not easy to degrade, and meanwhile, zinc is easy to deposit on the surface of sliding steel to form a stable and continuous protective layer, and meanwhile, the composite lubricating material also plays a role of an anti-seizing agent.
According to the invention, boric acid and zinc nitrate are synthesized into boric acid nano particles, if the boric acid nano particles are directly added by the solution, the solution is quickly evaporated under the conditions of high temperature and high pressure of microwaves, so that the synthesis and the formation of zinc borate are affected, meanwhile, the zinc borate particle dispersion solution is mixed with MOF synthetic solution in a dropwise adding mode, the zinc borate is dispersed in the MOF synthetic solution, the phenomenon of precipitation is avoided, and the slow addition has small influence on the combination of metal ions and ligands of MOF. Meanwhile, the positive charges on the surface of the zinc borate are more than those of other borates, the electrostatic attraction between the zinc borate and the MOF is stronger, and the zinc borate cannot fall off and deposit to the bottom in the dispersing process, so that the dispersion stability of the prepared lubricating material is better.
It should be noted that the above embodiments are only for illustrating the technical solution of the present invention and not for limiting the same, and although the present invention has been described in detail with reference to the preferred embodiments, it should be understood by those skilled in the art that the technical solution of the present invention may be modified or substituted without departing from the spirit and scope of the technical solution of the present invention, which is intended to be covered in the scope of the claims of the present invention.
Claims (1)
1. A preparation method of a zinc borate/Fe-BDC nano composite lubricating oil additive is characterized by comprising the following steps: comprises mixing 0.834g FeSO 4 ·7H 2 O and 0.420g of 1,3, 5-benzene tricarboxylic acid are dissolved in 60mL of N, N-dimethylformamide, and stirred until the mixture is completely dissolved, thus obtaining a mixed solution A;
respectively dissolving 10g of borax and 13g of zinc nitrate in deionized water, and stirring to form borax solution and zinc nitrate solution;
mixing and stirring the two solutions at 60 ℃ for 3 hours to form milky turbid liquid, and drying after suction filtration to synthesize zinc borate nano particles;
dispersing 5g of zinc borate particles in 10mL of deionized water to form uniformly dispersed zinc borate solution;
dripping zinc borate solution into the mixed solution A at the frequency of 2 drops/min, stirring, and performing ultrasonic treatment with the power of 350W for 20min until the zinc borate is completely dispersed;
after the solution is completely dispersed, placing the solution in a microwave oven for microwave hydrothermal synthesis for 4 minutes, wherein the microwave frequency is set to be 2.45GHz, and the power is set to be 300W;
and filtering the solution, washing and drying to obtain the product.
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