CN117285836A - Preparation method and application of melamine-formaldehyde modified Mxene - Google Patents
Preparation method and application of melamine-formaldehyde modified Mxene Download PDFInfo
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- CN117285836A CN117285836A CN202311128739.6A CN202311128739A CN117285836A CN 117285836 A CN117285836 A CN 117285836A CN 202311128739 A CN202311128739 A CN 202311128739A CN 117285836 A CN117285836 A CN 117285836A
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- 229920000877 Melamine resin Polymers 0.000 title claims abstract description 95
- IVJISJACKSSFGE-UHFFFAOYSA-N formaldehyde;1,3,5-triazine-2,4,6-triamine Chemical compound O=C.NC1=NC(N)=NC(N)=N1 IVJISJACKSSFGE-UHFFFAOYSA-N 0.000 title claims abstract description 75
- 238000002360 preparation method Methods 0.000 title claims abstract description 27
- PQXKHYXIUOZZFA-UHFFFAOYSA-M lithium fluoride Chemical compound [Li+].[F-] PQXKHYXIUOZZFA-UHFFFAOYSA-M 0.000 claims abstract description 32
- 238000001914 filtration Methods 0.000 claims abstract description 20
- 239000002253 acid Substances 0.000 claims abstract description 7
- 238000003756 stirring Methods 0.000 claims description 52
- 238000001035 drying Methods 0.000 claims description 31
- 239000000243 solution Substances 0.000 claims description 27
- 239000006185 dispersion Substances 0.000 claims description 24
- 239000007788 liquid Substances 0.000 claims description 22
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 20
- 239000008367 deionised water Substances 0.000 claims description 18
- 229910021641 deionized water Inorganic materials 0.000 claims description 18
- 238000006243 chemical reaction Methods 0.000 claims description 16
- JDSHMPZPIAZGSV-UHFFFAOYSA-N melamine Chemical compound NC1=NC(N)=NC(N)=N1 JDSHMPZPIAZGSV-UHFFFAOYSA-N 0.000 claims description 16
- UQZIWOQVLUASCR-UHFFFAOYSA-N alumane;titanium Chemical compound [AlH3].[Ti] UQZIWOQVLUASCR-UHFFFAOYSA-N 0.000 claims description 14
- WSFSSNUMVMOOMR-UHFFFAOYSA-N Formaldehyde Chemical compound O=C WSFSSNUMVMOOMR-UHFFFAOYSA-N 0.000 claims description 13
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 12
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims description 12
- 239000008098 formaldehyde solution Substances 0.000 claims description 10
- 239000000843 powder Substances 0.000 claims description 10
- 239000002244 precipitate Substances 0.000 claims description 10
- 230000001105 regulatory effect Effects 0.000 claims description 10
- 238000009210 therapy by ultrasound Methods 0.000 claims description 10
- 238000005406 washing Methods 0.000 claims description 9
- SECXISVLQFMRJM-UHFFFAOYSA-N N-Methylpyrrolidone Chemical compound CN1CCCC1=O SECXISVLQFMRJM-UHFFFAOYSA-N 0.000 claims description 8
- 239000002798 polar solvent Substances 0.000 claims description 8
- UIIMBOGNXHQVGW-UHFFFAOYSA-M Sodium bicarbonate Chemical compound [Na+].OC([O-])=O UIIMBOGNXHQVGW-UHFFFAOYSA-M 0.000 claims description 6
- 229910000029 sodium carbonate Inorganic materials 0.000 claims description 6
- 235000017550 sodium carbonate Nutrition 0.000 claims description 6
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims description 5
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 5
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims description 4
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 4
- 238000001291 vacuum drying Methods 0.000 claims description 4
- 235000017557 sodium bicarbonate Nutrition 0.000 claims description 3
- 229910000030 sodium bicarbonate Inorganic materials 0.000 claims description 3
- FXHOOIRPVKKKFG-UHFFFAOYSA-N N,N-Dimethylacetamide Chemical compound CN(C)C(C)=O FXHOOIRPVKKKFG-UHFFFAOYSA-N 0.000 claims description 2
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 2
- 239000003929 acidic solution Substances 0.000 claims description 2
- 229910017604 nitric acid Inorganic materials 0.000 claims description 2
- 239000007787 solid Substances 0.000 claims description 2
- 238000000034 method Methods 0.000 claims 6
- 238000000227 grinding Methods 0.000 abstract description 10
- 238000011065 in-situ storage Methods 0.000 abstract description 4
- 238000006116 polymerization reaction Methods 0.000 abstract description 4
- 230000002194 synthesizing effect Effects 0.000 abstract description 3
- 238000013329 compounding Methods 0.000 abstract description 2
- CAVCGVPGBKGDTG-UHFFFAOYSA-N alumanylidynemethyl(alumanylidynemethylalumanylidenemethylidene)alumane Chemical compound [Al]#C[Al]=C=[Al]C#[Al] CAVCGVPGBKGDTG-UHFFFAOYSA-N 0.000 abstract 1
- LEJBBGNFPAFPKQ-UHFFFAOYSA-N 2-(2-prop-2-enoyloxyethoxy)ethyl prop-2-enoate Chemical compound C=CC(=O)OCCOCCOC(=O)C=C LEJBBGNFPAFPKQ-UHFFFAOYSA-N 0.000 description 16
- -1 acrylic ester Chemical class 0.000 description 16
- 239000000203 mixture Substances 0.000 description 11
- 239000004593 Epoxy Substances 0.000 description 8
- 239000003795 chemical substances by application Substances 0.000 description 8
- 239000002270 dispersing agent Substances 0.000 description 8
- 239000004814 polyurethane Substances 0.000 description 8
- 229920002635 polyurethane Polymers 0.000 description 8
- 239000000080 wetting agent Substances 0.000 description 8
- 239000002518 antifoaming agent Substances 0.000 description 6
- 239000000463 material Substances 0.000 description 6
- 230000017525 heat dissipation Effects 0.000 description 5
- 238000007639 printing Methods 0.000 description 5
- 239000000047 product Substances 0.000 description 5
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 3
- 239000011159 matrix material Substances 0.000 description 3
- 238000011160 research Methods 0.000 description 3
- 238000006467 substitution reaction Methods 0.000 description 3
- 229910052582 BN Inorganic materials 0.000 description 2
- PZNSFCLAULLKQX-UHFFFAOYSA-N Boron nitride Chemical compound N#B PZNSFCLAULLKQX-UHFFFAOYSA-N 0.000 description 2
- 239000013530 defoamer Substances 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 239000000945 filler Substances 0.000 description 2
- 229910021389 graphene Inorganic materials 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- 206010063385 Intellectualisation Diseases 0.000 description 1
- 238000009825 accumulation Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 238000004220 aggregation Methods 0.000 description 1
- 239000012752 auxiliary agent Substances 0.000 description 1
- 239000011230 binding agent Substances 0.000 description 1
- 239000002041 carbon nanotube Substances 0.000 description 1
- 229910021393 carbon nanotube Inorganic materials 0.000 description 1
- 239000011231 conductive filler Substances 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000010419 fine particle Substances 0.000 description 1
- 239000012767 functional filler Substances 0.000 description 1
- 239000011256 inorganic filler Substances 0.000 description 1
- 229910003475 inorganic filler Inorganic materials 0.000 description 1
- 230000010354 integration Effects 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 239000002113 nanodiamond Substances 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 238000001878 scanning electron micrograph Methods 0.000 description 1
- 230000005476 size effect Effects 0.000 description 1
- 239000010936 titanium Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D11/00—Inks
- C09D11/02—Printing inks
- C09D11/03—Printing inks characterised by features other than the chemical nature of the binder
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D11/00—Inks
- C09D11/02—Printing inks
- C09D11/10—Printing inks based on artificial resins
- C09D11/101—Inks specially adapted for printing processes involving curing by wave energy or particle radiation, e.g. with UV-curing following the printing
-
- 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 provides a preparation method and application of melamine-formaldehyde modified Mxene, which comprises the steps of firstly synthesizing a melamine-formaldehyde prepolymer, then stripping aluminum carbide through a lithium fluoride acid solution to prepare the Mxene, finally carrying out in-situ polymerization on the melamine-formaldehyde prepolymer and the stripped Mxene to obtain the melamine-formaldehyde modified Mxene, compounding the melamine-formaldehyde modified Mxene with each component of the ink, grinding and filtering to obtain the high-efficiency heat conduction UV-LED ink.
Description
The application is a divisional application, the application number of the original application is 2021115569725, the application date is 2021, 12 months and 18 days, and the invention is named as a preparation method and application of the high-efficiency heat-conducting UV-LED ink.
Technical Field
The invention belongs to the technical field of high polymer ink, and particularly relates to a preparation method and application of melamine-formaldehyde modified Mxene.
Background
With the increasing maturity of 5G technology, electronic devices are gradually developed toward miniaturization, high integration and intellectualization, and thus the problem of heat accumulation becomes a key factor affecting the lifetime of electronic devices. Numerous studies have shown that, within a suitable operating temperature range, the occurrence of faults is reduced by 4% for every 1 ℃ drop in the operating temperature of the electronic device; when it is 20 ℃ above the maximum set temperature, the failure rate is as high as 100%. Therefore, development of high-performance heat dissipation materials is an important subject in the current application field of electronic devices.
Many scholars and research institutions conduct extensive researches on heat dissipation materials, such as graphene, boron nitride, aluminum oxide, carbon nanotubes, nano diamond and other heat conduction materials, are developed and applied to heat dissipation of electronic products successively, and good research results are achieved. However, focusing on commercialization of electronic products, it is not difficult to find that people tend to ignore another important problem: the outside of the electronic product is printed with ink to identify information. When the ink is printed on the surface of an electronic product and dried, a compact ink layer is formed, and the binder in the ink is solidified into a film and firmly attached to the surface of the electronic device, so that heat dissipation is prevented. Therefore, developing a functional ink which can not only meet the printing requirements of electronic products, but also timely emit heat becomes an important task at present. In this case, a thermally conductive ink is produced. The heat-conducting ink is prepared by adding a filler or an auxiliary agent with heat-conducting property on the basis of the traditional ink so as to endow the ink with excellent heat-conducting property. Compared with the traditional ink, the UV-LED ink is high in curing speed and low in energy consumption, and is combined with the heat-conducting filler, so that the novel heat-conducting ink with high efficiency and quick drying is expected to be developed.
Among the numerous thermally conductive fillers, graphene has a thermal conductivity as high as 5300W/m·k, but is costly and has been widely studied. The materials such as boron nitride and aluminum oxide have large addition amount when preparing the heat-conducting ink, and the basic performance of the ink can be affected. In contrast, the michael (Mxene) is a novel two-dimensional material, has significant advantages of being peelable, high in heat conductivity, unique in size effect, strong in heat dissipation capability and the like, and the raw material titanium aluminum carbide (Ti 3AlC 2) MAX is low in cost, so that the michael is a new material in the heat conduction field, and brings wide attention to academia and enterprise industries. However, mxene is an inorganic filler, and when it is directly added to an ink matrix, it tends to have problems such as poor compatibility and difficulty in dispersion, and thus the heat conductive property of the heat conductive ink generally prepared is not ideal.
Disclosure of Invention
Aiming at the problem of poor compatibility of Michael (Mxene) and an ink matrix, the invention provides a preparation method and application of melamine-formaldehyde modified Mxene.
The preparation method of the melamine-formaldehyde modified Mxene is applied to heat-conducting ink, and the melamine-formaldehyde modified Mxene is prepared by the following steps: synthesizing a melamine-formaldehyde prepolymer, stripping titanium aluminum carbide by a lithium fluoride acid solution to prepare Mxene, and carrying out in-situ polymerization on the melamine-formaldehyde prepolymer and the stripped Mxene to obtain the melamine-formaldehyde modified Mxene.
The principle of the invention is as follows:
by utilizing the in-situ polymerization of the melamine-formaldehyde resin to the Mxene, the aggregation of the Mxene is effectively reduced, the dispersibility of the Mxene in the ink is improved, and the heat conductivity coefficient of the ink is greatly increased.
The melamine-formaldehyde modified Mxene is prepared by the steps of:
(1) Adding melamine into a polar solution, uniformly stirring, setting the temperature to be 50-80 ℃, slowly adding formaldehyde solution with the mass fraction of 30-40%, regulating the pH to be 7-10 by weak base, reacting for 1-2 hours, continuously maintaining stirring for 30-60 minutes after the reaction is finished, and standing to obtain melamine-formaldehyde prepolymer;
(2) Adding lithium fluoride into an acidic solution, stirring and dissolving, adding titanium aluminum carbide powder, stirring and reacting for 4-48 hours at 30-60 ℃, washing with deionized water until the pH is between 5-9, placing in an ultrasonic cleaner, performing ultrasonic stripping for 5-60 minutes, setting the power to be 100-400W, centrifuging the reaction solution for 10-30 minutes at 1000-10000r/min after stripping is finished, and placing the lower precipitate in a drying box for drying to obtain Mxene;
(3) Adding Mxene into a polar solvent, carrying out ultrasonic treatment for 30-90 minutes at 30-80 ℃ to obtain Mxene dispersion liquid, adding the Mxene dispersion liquid into the melamine-formaldehyde prepolymer prepared in the step (1), stirring for 4-8 hours, setting the temperature to 50-100 ℃, the stirring speed to 300-1000r/min, filtering, and carrying out vacuum drying to obtain the melamine-formaldehyde modified Mxene.
The preparation method of the melamine-formaldehyde modified Mxene comprises the following steps of: 5-10.
The preparation method of the melamine-formaldehyde modified Mxene comprises the following steps of: 1-10.
The preparation method of the melamine-formaldehyde modified Mxene comprises the following steps of: 1-20.
The preparation method of the melamine-formaldehyde modified Mxene comprises the following steps (1):
the polar solvent is water;
the solid content of the melamine is 5-30% after the melamine is added into the polar solvent;
the weak base is one of sodium carbonate, sodium bicarbonate or ammonia water.
The preparation method of the melamine-formaldehyde modified Mxene comprises the following steps: in the step (2):
the acid solution is one of hydrochloric acid, sulfuric acid or nitric acid;
the concentration of the lithium fluoride acid solution is 1.00-20.00mg/ml.
The preparation method of the melamine-formaldehyde modified Mxene comprises the following steps:
the polar solvent is one of N, N-dimethylacetamide, N-methylpyrrolidone or isopropanol;
the concentration of the Mxene dispersion liquid is 0.08-10mg/ml;
the power of the ultrasonic wave is 100-325W;
the vacuum drying condition is preferably drying for 4-20 hours at 25-100 ℃.
The melamine-formaldehyde modified Mxene prepared by the preparation method is applied to heat-conducting ink.
Compared with the prior art, the invention has the following advantages:
the invention provides a preparation method of melamine-formaldehyde modified Mxene, which comprises the steps of firstly synthesizing a melamine-formaldehyde prepolymer, then stripping titanium aluminum carbide through a lithium fluoride acid solution to prepare Mxene, finally carrying out in-situ polymerization on the melamine-formaldehyde prepolymer and stripped Mxene to obtain the melamine-formaldehyde modified Mxene, compounding the melamine-formaldehyde modified Mxene with each component of the ink, grinding and filtering to obtain the high-efficiency heat conduction UV-LED ink.
The invention solves the problems of poor compatibility, difficult dispersion and the like of the Mxene added into an ink matrix, the prepared heat-conducting functional filler has the advantages of small addition amount and good heat-conducting effect, the heat conductivity coefficient of the ink is greatly improved, and the preparation method of the high-efficiency heat-conducting UV-LED ink is simple in preparation process and strong in operability.
Drawings
In order to more clearly illustrate the technical solutions in the embodiments of the present application, the drawings that are required to be used in the description of the embodiments will be briefly described below.
FIG. 1 is an SEM image of Mxene and melamine-formaldehyde resin modified Mxene.
FIG. 2 is an infrared plot of the melamine-formaldehyde resin modified Mxene prepared in example 5.
FIG. 3 is a graph of thermal conductivity measurements of the high efficiency thermal conductivity UV-LED ink prepared in example 5.
Detailed Description
The following describes the specific technical scheme of the present invention with reference to specific examples 1 to 8:
example 1
A preparation method of high-efficiency heat-conducting UV-LED ink comprises the following steps:
(1) Adding 60mL of deionized water into 6g of melamine, and stirring at a rotating speed of 300r/min; then, 14mL (37%) of formaldehyde solution is dripped, the pH is regulated to 9 by using a newly prepared Na2CO3 (10%) solution, the temperature is raised to 80 ℃, and stirring is continued for 20 minutes, so as to obtain a melamine-formaldehyde prepolymer;
(2) 1.0g of lithium fluoride is added with 150mL of HCl and stirred for 5 minutes, then 2.0g of titanium aluminum carbide powder is added, the mixture is stirred and reacted for 8 hours at 30 ℃, deionized water is used for washing to pH 5.5, and the mixture is placed in an ultrasonic cleaner for ultrasonic stripping for 10 minutes, and the power is set to be 200w. After stripping is finished, centrifuging the reaction solution for 10 minutes under the condition of 2000r/min, taking the precipitate at the lower layer, and drying in a drying oven to obtain Mxene;
(3) Taking 1.0g of Mxene, adding 300mL of N-methylpyrrolidone, carrying out ultrasonic treatment at 50 ℃ for 40 minutes and with the power of 250w to obtain Mxene dispersion liquid, adding the Mxene dispersion liquid into the melamine-formaldehyde prepolymer prepared in the step (1), stirring for 3 hours, setting the temperature to 50 ℃, the stirring speed to 350r/min, and drying at 80 ℃ for 2 hours after filtering to obtain melamine-formaldehyde modified Mxene (MF@Mxene);
(4) And (3) adding melamine-formaldehyde modified Mxene (MF@Mxene), polyurethane acrylic ester, epoxy acrylic ester, diethylene glycol diacrylate, a photoinitiator, a leveling agent, a defoaming agent, a dispersing agent and a wetting agent which are prepared in the step (3) into a high-speed dispersing machine according to the proportion of 0.5%, 35%, 15%, 35%, 8%, 2%, 1% and 2.5% relative to the total mass of the ink, dispersing for 2 hours under the condition of 2000r/min, then crushing and grinding for 3 hours by a three-roller machine, and finally filtering by a 300-mesh screen, thereby preparing the high-efficiency heat-conducting UV-LED heat-conducting ink.
Example 2
A preparation method of high-efficiency heat-conducting UV-LED ink comprises the following steps:
(1) Adding 40mL of deionized water into 4g of melamine, and stirring at a rotating speed of 200r/min; then 7.2mL (37%) of formaldehyde solution is dripped, the pH is regulated to 8 by using a newly prepared Na2CO3 (10%) solution, the temperature is raised to 70 ℃, and stirring is continued for 30 minutes, so as to obtain melamine-formaldehyde prepolymer;
(2) 1.5g of lithium fluoride is added with 200mL of HCl and stirred for 10 minutes, then 2.5g of titanium aluminum carbide powder is added, and the mixture is stirred and reacted for 10 hours at 40 ℃, washed with deionized water until the pH is 6, and then the mixture is placed in an ultrasonic cleaner for ultrasonic stripping for 15 minutes, and the power is set to be 200w. After stripping is finished, centrifuging the reaction solution for 15 minutes under the condition of 2500r/min, taking the precipitate at the lower layer, and drying in a drying oven to obtain Mxene;
(3) Taking 1.5g of Mxene, adding 500mL of N-methylpyrrolidone, carrying out ultrasonic treatment at 40 ℃ for 60 minutes and with the power of 100w to obtain Mxene dispersion liquid, adding the Mxene dispersion liquid into the melamine-formaldehyde prepolymer prepared in the step (1), stirring for 4 hours, setting the temperature to 50 ℃, the stirring speed to 400r/min, and drying at 60 ℃ for 8 hours after filtering to obtain melamine-formaldehyde modified Mxene (MF@Mxene);
(4) And (3) adding the melamine-formaldehyde modified Mxene (MF@Mxene), polyurethane acrylic ester, epoxy acrylic ester, diethylene glycol diacrylate, a photoinitiator, a leveling agent, a defoaming agent, a dispersing agent and a wetting agent which are prepared in the step (3) into a high-speed dispersing machine according to the proportion of 1%, 35%, 10%, 45%, 3%, 2%, 1% and 2% relative to the total mass of the ink, dispersing for 1 hour under the condition of 4000r/min, then crushing and grinding for 1 hour by a three-roller machine, and finally filtering by a 200-mesh screen, thereby preparing the high-efficiency heat-conducting UV-LED heat-conducting ink.
Example 3
A preparation method of high-efficiency heat-conducting UV-LED ink comprises the following steps:
(1) Adding 35mL of deionized water into 3g of melamine, and stirring at the rotating speed of 250r/min; then 7.5mL (37%) of formaldehyde solution is dripped, the pH is regulated to 10 by using a newly prepared Na2CO3 (10%) solution, the temperature is raised to 60 ℃, and stirring is continued for 40 minutes, so as to obtain a melamine-formaldehyde prepolymer;
(2) 2.0g of lithium fluoride is taken, 400mL of HCl is added, stirring is carried out for 15 minutes, then 5g of titanium aluminum carbide powder is added, stirring reaction is carried out for 15 hours at 40 ℃, deionized water is used for washing to pH 7, the mixture is placed in an ultrasonic cleaner for ultrasonic stripping for 20 minutes, and the power is set to 300w. After stripping is finished, centrifuging the reaction solution for 10 minutes at 3000r/min, taking the precipitate at the lower layer, and drying in a drying oven to obtain Mxene;
(3) Adding 450 mLN-methylpyrrolidone into 4g of Mxene, carrying out ultrasonic treatment at 60 ℃ for 30 minutes and with the power of 150w to obtain Mxene dispersion liquid, adding the Mxene dispersion liquid into the melamine-formaldehyde prepolymer prepared in the step (1), stirring for 2 hours, setting the temperature to 60 ℃, the stirring speed to 300r/min, and drying at 70 ℃ for 6 hours after filtering to obtain melamine-formaldehyde modified Mxene (MF@Mxene);
(4) And (3) adding the melamine-formaldehyde modified Mxene (MF@Mxene), polyurethane acrylic ester, epoxy acrylic ester, diethylene glycol diacrylate, a photoinitiator, a leveling agent, a defoaming agent, a dispersing agent and a wetting agent which are prepared in the step (3) into a high-speed dispersing machine according to the proportion of 1.5%, 20%, 25%, 40%, 6%, 3.5%, 1.5%, 2% and 0.5% relative to the total mass of the ink, dispersing for 2 hours under the condition of 3000r/min, grinding for 2 hours by a three-roller machine, and filtering by a 200-mesh screen to obtain the high-efficiency heat-conducting UV-LED heat-conducting ink.
Example 4
A preparation method of high-efficiency heat-conducting UV-LED ink comprises the following steps:
(1) Adding 30mL of deionized water into 10g of melamine, and stirring at a rotating speed of 300r/min; then 18.9mL (37%) of formaldehyde solution is added dropwise, the PH is regulated to 10 by using a newly prepared NaHCO3 (10%) solution, the temperature is raised to 70 ℃, and stirring is continued for 40 minutes, so as to obtain melamine-formaldehyde prepolymer;
(2) 2.5g of lithium fluoride is taken, 400mL of HCl is added, stirring is carried out for 20 minutes, then 6g of titanium aluminum carbide powder is added, stirring reaction is carried out for 20 hours at 50 ℃, deionized water is used for washing to pH 8, the mixture is placed in an ultrasonic cleaner for ultrasonic stripping for 30 minutes, and the power is set to 300w. After stripping is finished, centrifuging the reaction solution for 20 minutes under 3500r/min, taking the precipitate at the lower layer, and drying in a drying oven to obtain Mxene;
(3) Taking 4.5g of Mxene, adding 450mL of N-methylpyrrolidone, carrying out ultrasonic treatment at 50 ℃ for 60 minutes and with the power of 350w to obtain Mxene dispersion liquid, adding the Mxene dispersion liquid into the melamine-formaldehyde prepolymer prepared in the step (1), stirring for 1 hour, setting the temperature to 40 ℃, the stirring speed to 300r/min, and drying for 3 hours at 70 ℃ after filtering to obtain melamine-formaldehyde modified Mxene (MF@Mxene);
(4) And (3) adding the melamine-formaldehyde modified Mxene (MF@Mxene), polyurethane acrylic ester, epoxy acrylic ester, diethylene glycol diacrylate, a photoinitiator, a leveling agent, a defoaming agent, a dispersing agent and a wetting agent which are prepared in the step (3) into a high-speed dispersing machine according to the proportion of 2%, 25%, 35%, 3%, 3.5%, 1%, 3.5% and 2% relative to the total mass of the ink, dispersing for 2 hours under the condition of 3500r/min, then crushing and grinding for 2 hours by a three-roller machine, and finally filtering by a 250-mesh gauze to obtain the high-efficiency heat-conducting UV-LED heat-conducting ink.
Example 5
A preparation method of high-efficiency heat-conducting UV-LED ink comprises the following steps:
(1) Adding 60mL of deionized water into 5g of melamine, and stirring at a rotating speed of 300r/min; then 8.9mL (37%) of formaldehyde solution is dripped, the pH is regulated to 10 by using a newly prepared Na2CO3 (10%) solution, the temperature is raised to 70 ℃, and stirring is continued for 60 minutes, so as to obtain melamine-formaldehyde prepolymer;
(2) 3.0g of lithium fluoride is taken, 500mL of HCl is added, stirring is carried out for 10 minutes, then 3.0g of titanium aluminum carbide powder is added, stirring reaction is carried out for 24 hours at 42 ℃, deionized water is used for washing to pH 6, the mixture is placed in an ultrasonic cleaner for ultrasonic stripping for 30 minutes, and the power is set to 300w. After stripping is finished, centrifuging the reaction solution for 30 minutes under 3500r/min, taking the precipitate at the lower layer, and drying in a drying oven to obtain Mxene;
(3) Adding 500mL of N-methylpyrrolidone into 1.0g of Mxene, carrying out ultrasonic treatment at 50 ℃ for 90 minutes and with the power of 325w to obtain Mxene dispersion liquid, adding the Mxene dispersion liquid into the melamine-formaldehyde prepolymer prepared in the step (1), stirring for 2 hours, setting the temperature to 50 ℃, the stirring speed to 300r/min, and drying at 80 ℃ for 3 hours after filtering to obtain melamine-formaldehyde modified Mxene (MF@Mxene);
(4) And (3) adding the melamine-formaldehyde modified Mxene (MF@Mxene), polyurethane acrylic ester, epoxy acrylic ester, diethylene glycol diacrylate, a photoinitiator, a leveling agent, a defoaming agent, a dispersing agent and a wetting agent which are prepared in the step (3) into a high-speed dispersing machine according to the proportion of 3%, 30%, 10%, 40%, 5%, 2%, 3%, 2% and 3% relative to the total mass of the printing ink, dispersing for 2 hours under the condition of 3000r/min, then crushing and grinding for 2 hours by a three-roller machine, and finally filtering by a 250-mesh screen, thereby preparing the high-efficiency heat-conducting UV-LED heat-conducting printing ink.
Example 6
A preparation method of high-efficiency heat-conducting UV-LED ink comprises the following steps:
(1) Adding 100mL of deionized water into 8g of melamine, and stirring at a rotating speed of 500r/min; then 15mL (37%) of formaldehyde solution is dripped, the pH is regulated to 10 by using newly prepared ammonia water (10%) solution, the temperature is raised to 60 ℃, and stirring is continued for 60 minutes, thus obtaining melamine-formaldehyde prepolymer;
(2) 4.0g of lithium fluoride is taken, 500mL of HCl is added, stirring is carried out for 15 minutes, then 6.0g of titanium aluminum carbide powder is added, stirring reaction is carried out for 18 hours at 45 ℃, deionized water is used for washing to pH 9, the mixture is placed in an ultrasonic cleaner for ultrasonic stripping for 30 minutes, and the power is set to 150w. After stripping is finished, centrifuging the reaction solution for 35 minutes under the condition of 4000r/min, taking the precipitate at the lower layer, and drying in a drying oven to obtain Mxene;
(3) Adding 500 mLN-methylpyrrolidone into 4.0g of Mxene, carrying out ultrasonic treatment at 60 ℃ for 40 minutes and with the power of 300w to obtain Mxene dispersion liquid, adding the Mxene dispersion liquid into the melamine-formaldehyde prepolymer prepared in the step (1), stirring for 2.5 hours, setting the temperature to 60 ℃, the stirring speed to 500r/min, filtering, and drying at 60 ℃ for 3 hours to obtain melamine-formaldehyde modified Mxene (MF@Mxene);
(4) And (3) adding the melamine-formaldehyde modified Mxene (MF@Mxene), polyurethane acrylic ester, epoxy acrylic ester, diethylene glycol diacrylate, a photoinitiator, a flatting agent, a defoamer, a dispersing agent and a wetting agent which are prepared in the step (3) into a high-speed dispersing machine according to the proportion of 5%, 35%, 15%, 30%, 8%, 3%, 0.5% and 0.5% relative to the total mass of the ink, dispersing for 2 hours under the condition of 3000r/min, then crushing and grinding for 3 hours by a three-roller machine, and finally filtering by a 500-mesh gauze to obtain the high-efficiency heat-conducting UV-LED heat-conducting ink.
Example 7
A preparation method of high-efficiency heat-conducting UV-LED ink comprises the following steps:
(1) Adding 90mL of deionized water into 6.5g of melamine, and stirring at a rotating speed of 800r/min; then 18mL (37%) of formaldehyde solution is dripped, the pH is regulated to 10 by using newly prepared ammonia water (10%) solution, the temperature is raised to 75 ℃, and stirring is continued for 50 minutes, thus obtaining melamine-formaldehyde prepolymer;
(2) 5.0g of lithium fluoride is added with 500mL of HCl and stirred for 30 minutes, then 6.0g of titanium aluminum carbide powder is added, the mixture is stirred and reacted for 36 hours at 50 ℃, deionized water is used for washing to pH 8, and the mixture is placed in an ultrasonic cleaner for ultrasonic stripping for 15 minutes, and the power is set to 250w. After stripping is finished, centrifuging the reaction solution for 35 minutes at 3000r/min, taking the precipitate at the lower layer, and drying in a drying oven to obtain Mxene;
(3) Adding 500mL of N-methylpyrrolidone into 5.0g of Mxene, carrying out ultrasonic treatment at 60 ℃ for 60 minutes and with the power of 300w to obtain Mxene dispersion liquid, adding the Mxene dispersion liquid into the melamine-formaldehyde prepolymer prepared in the step (1), stirring for 3 hours, setting the temperature to 60 ℃, the stirring speed to 300r/min, and drying at 50 ℃ for 2 hours after filtering to obtain melamine-formaldehyde modified Mxene (MF@Mxene);
(4) And (3) adding melamine-formaldehyde modified Mxene (MF@Mxene), polyurethane acrylic ester, epoxy acrylic ester, diethylene glycol diacrylate, a photoinitiator, a flatting agent, a defoamer, a dispersing agent and a wetting agent which are prepared in the step (3) into a high-speed dispersing machine according to the proportion of 6%, 30%, 15%, 35%, 4%, 3%, 2%, 2.5% and 2.5% relative to the total mass of the ink, dispersing for 2 hours under the condition of 5000r/min, then crushing and grinding for 1 hour by a three-roller machine, and finally filtering by a 800-mesh gauze to obtain the high-efficiency heat-conducting UV-LED heat-conducting ink.
Example 8
A preparation method of high-efficiency heat-conducting UV-LED ink comprises the following steps:
(1) Adding 120mL of deionized water into 7g of melamine, and stirring at a rotating speed of 600r/min; then 20mL (37%) of formaldehyde solution is dripped, the pH is regulated to 9 by using newly prepared ammonia water (10%) solution, the temperature is raised to 80 ℃, and stirring is continued for 60 minutes, thus obtaining melamine-formaldehyde prepolymer;
(2) 6.0g of lithium fluoride is added into 800mL of HCl, stirred for 40 minutes, then 6.0g of titanium aluminum carbide powder is added, stirred and reacted for 40 hours at 60 ℃, deionized water is used for washing to pH 7, and the mixture is placed in an ultrasonic cleaner for ultrasonic stripping for 25 minutes, and the power is set to 300w. After stripping is finished, centrifuging the reaction solution for 30 minutes under 3500r/min, taking the precipitate at the lower layer, and drying in a drying oven to obtain Mxene;
(3) Taking 5.0g of Mxene, adding 350mL of N-methylpyrrolidone, carrying out ultrasonic treatment at 80 ℃ for 40 minutes and with the power of 300w to obtain Mxene dispersion liquid, adding the Mxene dispersion liquid into the melamine-formaldehyde prepolymer prepared in the step (1), stirring for 2 hours, setting the temperature to 70 ℃, the stirring speed to 300r/min, and drying for 2 hours at 80 ℃ after filtering to obtain melamine-formaldehyde modified Mxene (MF@Mxene);
(4) And (3) adding the melamine-formaldehyde modified Mxene (MF@Mxene), polyurethane acrylic ester, epoxy acrylic ester, diethylene glycol diacrylate, a photoinitiator, a leveling agent, a defoaming agent, a dispersing agent and a wetting agent which are prepared in the step (3) into a high-speed dispersing machine according to the proportion of 7%, 35%, 13%, 35%, 8%, 0.5% and 0.5% relative to the total mass of the printing ink, dispersing for 2 hours under the condition of 6000r/min, grinding for 1.5 hours by a three-roller machine, and finally filtering by a 800-mesh screen to prepare the high-efficiency heat-conducting UV-LED heat-conducting printing ink.
Effect examples
The raw material Mxene and the intermediate melamine-formaldehyde functionalized Mxene in example 1 were subjected to electron microscopic scanning, and as can be seen from the scanning electron microscopic picture (fig. 1), compared with Mxene, mxene after being embedded with melamine-formaldehyde resin had a very rough surface, and a lot of fine particles were significantly loaded.
Meanwhile, the high-efficiency heat conduction UV-LED heat conduction ink prepared in the examples 1-8 is subjected to in-plane heat conduction coefficient test, and compared with the heat conduction ink reported in the prior art (Table 1), the high-efficiency heat conduction UV-LED heat conduction ink prepared in the invention has the heat conduction coefficient obviously higher than that of the heat conduction ink reported in the prior art under the condition of extremely low addition amount as shown in the Table 1.
Table 1 thermal conductivity comparison
As can be seen from the test data in Table 1, the high-efficiency heat-conducting UV-LED ink of the present application has a small amount of melamine-formaldehyde modified Mxene, which can greatly improve the heat conductivity of the ink, and the heat conductivity of the printed ink film is as high as 1.32W/mK in the plane direction when the heat conductivity is only 3.0wt%, and the embodiment 5 is a preferred embodiment of the present invention, but the embodiment of the present invention is not limited by the embodiment, and any other changes, modifications, substitutions, combinations, and simplifications which do not deviate from the spirit and principle of the present invention should be equivalent substitution modes, and all the changes, modifications, substitutions, combinations, and simplifications are included in the protection scope of the present invention.
Claims (8)
1. The preparation method of the melamine-formaldehyde modified Mxene, which is applied to the heat-conducting ink, is characterized by comprising the following steps of:
(1) Adding melamine into a polar solution, uniformly stirring, setting the temperature to be 50-80 ℃, slowly adding formaldehyde solution with the mass fraction of 30-40%, regulating the pH to be 7-10 by weak base, reacting for 1-2 hours, continuously maintaining stirring for 30-60 minutes after the reaction is finished, and standing to obtain melamine-formaldehyde prepolymer;
(2) Adding lithium fluoride into an acidic solution, stirring and dissolving, adding titanium aluminum carbide powder, stirring and reacting for 4-48 hours at 30-60 ℃, washing with deionized water until the pH is between 5-9, placing in an ultrasonic cleaner, performing ultrasonic stripping for 5-60 minutes, setting the power to be 100-400W, centrifuging the reaction solution for 10-30 minutes at 1000-10000r/min after stripping is finished, and placing the lower precipitate in a drying box for drying to obtain Mxene;
(3) Adding Mxene into a polar solvent, carrying out ultrasonic treatment for 30-90 minutes at 30-80 ℃ to obtain Mxene dispersion liquid, adding the Mxene dispersion liquid into the melamine-formaldehyde prepolymer prepared in the step (1), stirring for 4-8 hours, setting the temperature to 50-100 ℃, the stirring speed to 300-1000r/min, filtering, and carrying out vacuum drying to obtain the melamine-formaldehyde modified Mxene.
2. The method for preparing the melamine-formaldehyde modified Mxene according to claim 1, characterized in that: the mole ratio of melamine to formaldehyde is 1:5-10.
3. The method for preparing the melamine-formaldehyde modified Mxene according to claim 1, characterized in that: the mass ratio of the lithium fluoride to the titanium aluminum carbide is 1:1-10.
4. The method for preparing the melamine-formaldehyde modified Mxene according to claim 1, characterized in that: the mass ratio of Mxene to melamine is 1:1-20.
5. The method for preparing the melamine-formaldehyde modified Mxene according to claim 1, characterized in that: in step (1):
the polar solvent is water;
the solid content of the melamine is 5-30% after the melamine is added into the polar solvent;
the weak base is one of sodium carbonate, sodium bicarbonate or ammonia water.
6. The method for preparing the melamine-formaldehyde modified Mxene according to claim 1, characterized in that: in the step (2):
the acid solution is one of hydrochloric acid, sulfuric acid or nitric acid;
the concentration of the lithium fluoride acid solution is 1.00-20.00mg/ml.
7. The method for preparing the melamine-formaldehyde modified Mxene according to claim 1, characterized in that:
in the step (3):
the polar solvent is one of N, N-dimethylacetamide, N-methylpyrrolidone or isopropanol;
the concentration of the Mxene dispersion liquid is 0.08-10mg/ml;
the power of the ultrasonic wave is 100-325W;
the vacuum drying condition is preferably drying for 4-20 hours at 25-100 ℃.
8. Use of melamine-formaldehyde modified Mxene prepared by the preparation method according to any of the claims 1-7 in a thermal ink.
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