CN113604105A - High-heat-dissipation ink and preparation method thereof - Google Patents
High-heat-dissipation ink and preparation method thereof Download PDFInfo
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- CN113604105A CN113604105A CN202110822030.0A CN202110822030A CN113604105A CN 113604105 A CN113604105 A CN 113604105A CN 202110822030 A CN202110822030 A CN 202110822030A CN 113604105 A CN113604105 A CN 113604105A
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- 238000002360 preparation method Methods 0.000 title claims abstract description 37
- 229920006335 epoxy glue Polymers 0.000 claims abstract description 58
- 239000000945 filler Substances 0.000 claims abstract description 47
- 239000002904 solvent Substances 0.000 claims abstract description 47
- TZCXTZWJZNENPQ-UHFFFAOYSA-L barium sulfate Chemical compound [Ba+2].[O-]S([O-])(=O)=O TZCXTZWJZNENPQ-UHFFFAOYSA-L 0.000 claims abstract description 41
- 239000002994 raw material Substances 0.000 claims abstract description 32
- 239000003822 epoxy resin Substances 0.000 claims abstract description 31
- 229920000647 polyepoxide Polymers 0.000 claims abstract description 31
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 30
- 239000003054 catalyst Substances 0.000 claims abstract description 28
- 239000002270 dispersing agent Substances 0.000 claims abstract description 28
- 239000002518 antifoaming agent Substances 0.000 claims abstract description 27
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 23
- 239000002041 carbon nanotube Substances 0.000 claims abstract description 23
- 229910021393 carbon nanotube Inorganic materials 0.000 claims abstract description 23
- LLHKCFNBLRBOGN-UHFFFAOYSA-N propylene glycol methyl ether acetate Chemical compound COCC(C)OC(C)=O LLHKCFNBLRBOGN-UHFFFAOYSA-N 0.000 claims abstract description 21
- POAOYUHQDCAZBD-UHFFFAOYSA-N 2-butoxyethanol Chemical compound CCCCOCCO POAOYUHQDCAZBD-UHFFFAOYSA-N 0.000 claims abstract description 7
- UYAAVKFHBMJOJZ-UHFFFAOYSA-N diimidazo[1,3-b:1',3'-e]pyrazine-5,10-dione Chemical compound O=C1C2=CN=CN2C(=O)C2=CN=CN12 UYAAVKFHBMJOJZ-UHFFFAOYSA-N 0.000 claims abstract description 7
- 229940116423 propylene glycol diacetate Drugs 0.000 claims abstract description 7
- 239000011259 mixed solution Substances 0.000 claims description 61
- 238000003756 stirring Methods 0.000 claims description 52
- 230000017525 heat dissipation Effects 0.000 claims description 31
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 28
- 239000004721 Polyphenylene oxide Substances 0.000 claims description 25
- 229920000570 polyether Polymers 0.000 claims description 25
- 229920005862 polyol Polymers 0.000 claims description 25
- 150000003077 polyols Chemical class 0.000 claims description 25
- DNIAPMSPPWPWGF-UHFFFAOYSA-N Propylene glycol Chemical compound CC(O)CO DNIAPMSPPWPWGF-UHFFFAOYSA-N 0.000 claims description 24
- LGRFSURHDFAFJT-UHFFFAOYSA-N Phthalic anhydride Natural products C1=CC=C2C(=O)OC(=O)C2=C1 LGRFSURHDFAFJT-UHFFFAOYSA-N 0.000 claims description 19
- JHIWVOJDXOSYLW-UHFFFAOYSA-N butyl 2,2-difluorocyclopropane-1-carboxylate Chemical compound CCCCOC(=O)C1CC1(F)F JHIWVOJDXOSYLW-UHFFFAOYSA-N 0.000 claims description 19
- LYCAIKOWRPUZTN-UHFFFAOYSA-N ethylene glycol Natural products OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 17
- 239000002253 acid Substances 0.000 claims description 16
- 239000003292 glue Substances 0.000 claims description 16
- 229920006332 epoxy adhesive Polymers 0.000 claims description 15
- 239000000377 silicon dioxide Substances 0.000 claims description 10
- -1 ethylene glycol siloxane Chemical class 0.000 claims description 9
- 238000001914 filtration Methods 0.000 claims description 9
- 238000000034 method Methods 0.000 claims description 9
- JOXIMZWYDAKGHI-UHFFFAOYSA-N toluene-4-sulfonic acid Chemical compound CC1=CC=C(S(O)(=O)=O)C=C1 JOXIMZWYDAKGHI-UHFFFAOYSA-N 0.000 claims description 9
- QTBSBXVTEAMEQO-UHFFFAOYSA-M Acetate Chemical compound CC([O-])=O QTBSBXVTEAMEQO-UHFFFAOYSA-M 0.000 claims description 8
- 238000001816 cooling Methods 0.000 claims description 8
- 238000010790 dilution Methods 0.000 claims description 8
- 239000012895 dilution Substances 0.000 claims description 8
- 238000010438 heat treatment Methods 0.000 claims description 8
- SNRUBQQJIBEYMU-UHFFFAOYSA-N Dodecane Natural products CCCCCCCCCCCC SNRUBQQJIBEYMU-UHFFFAOYSA-N 0.000 claims description 3
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical group C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 claims description 3
- USIUVYZYUHIAEV-UHFFFAOYSA-N diphenyl ether Chemical compound C=1C=CC=CC=1OC1=CC=CC=C1 USIUVYZYUHIAEV-UHFFFAOYSA-N 0.000 claims description 3
- 125000003438 dodecyl group Chemical group [H]C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])* 0.000 claims description 3
- PSHKMPUSSFXUIA-UHFFFAOYSA-N n,n-dimethylpyridin-2-amine Chemical compound CN(C)C1=CC=CC=N1 PSHKMPUSSFXUIA-UHFFFAOYSA-N 0.000 claims description 3
- 229910052708 sodium Inorganic materials 0.000 claims description 3
- 239000011734 sodium Substances 0.000 claims description 3
- 239000000853 adhesive Substances 0.000 abstract description 10
- 230000001070 adhesive effect Effects 0.000 abstract description 10
- 230000003287 optical effect Effects 0.000 abstract description 7
- 239000000126 substance Substances 0.000 abstract description 3
- 235000012239 silicon dioxide Nutrition 0.000 description 8
- 239000005543 nano-size silicon particle Substances 0.000 description 6
- ZIWRUEGECALFST-UHFFFAOYSA-M sodium 4-(4-dodecoxysulfonylphenoxy)benzenesulfonate Chemical group [Na+].CCCCCCCCCCCCOS(=O)(=O)c1ccc(Oc2ccc(cc2)S([O-])(=O)=O)cc1 ZIWRUEGECALFST-UHFFFAOYSA-M 0.000 description 6
- 238000004519 manufacturing process Methods 0.000 description 5
- 230000009257 reactivity Effects 0.000 description 4
- 238000009825 accumulation Methods 0.000 description 3
- 238000000576 coating method Methods 0.000 description 3
- 230000000052 comparative effect Effects 0.000 description 3
- 238000005260 corrosion Methods 0.000 description 3
- 230000007797 corrosion Effects 0.000 description 3
- 230000008569 process Effects 0.000 description 3
- 239000011248 coating agent Substances 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 239000002390 adhesive tape Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000005336 cracking Methods 0.000 description 1
- 239000013530 defoamer Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000001804 emulsifying effect Effects 0.000 description 1
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 230000036314 physical performance Effects 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 238000009736 wetting Methods 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
- C09D11/10—Printing inks based on artificial resins
- C09D11/102—Printing inks based on artificial resins containing macromolecular compounds obtained by reactions other than those only involving unsaturated carbon-to-carbon bonds
-
- 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
Landscapes
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Wood Science & Technology (AREA)
- Organic Chemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Inks, Pencil-Leads, Or Crayons (AREA)
- Adhesives Or Adhesive Processes (AREA)
Abstract
The invention discloses high-heat-dissipation ink which comprises the following preparation raw materials in parts by weight: 30-50 parts of modified epoxy glue, 15-25 parts of solvent, 10-20 parts of curing agent, 10-20 parts of filler, 0.5-3 parts of catalyst, 0.5-1 part of dispersing agent, 2-7 parts of defoaming agent and 0.1-2 parts of carbon nano tube; the modified epoxy glue at least comprises epoxy resin, and the volume of the epoxy resin accounts for 20-50% of the volume of the modified epoxy glue; wherein, the solvent comprises one or more of propylene glycol methyl ether acetate, ethylene glycol monobutyl ether and propylene glycol diacetate; the filler comprises at least nano barium sulfate. Correspondingly, the invention also provides a preparation method of the high-thermal-conductivity ink. The high-heat-dissipation ink obtained by the proportioning is obtained by mutual reaction of various raw materials, has strong adhesive force and chemical resistance, and improves the wear resistance of the ink by adding the filler on the premise of not influencing the optical performance of the ink.
Description
Technical Field
The invention relates to the technical field of circuit board coatings, in particular to high-heat-dissipation ink, and correspondingly relates to a preparation method of the ink.
Background
With the widespread application of electronic informatization, the PCB is widely applied to various devices, and the PCB mainly functions to mount various electronic components, and when the PCB is applied to the fields of display screens and the like, the PCB is required to have high heat dissipation performance and optical performance.
However, when the PCB is applied to a product with a large heat value, such as a display screen, the adhesion of the ink is affected due to heat accumulation, so that the ink is peeled off and foamed, and the overall optical performance of the PCB is affected.
Disclosure of Invention
The invention aims to solve the technical problem of providing the high-heat-dissipation ink which is strong in adhesive force, good in heat dissipation performance and especially suitable for equipment with large heat productivity.
The invention also aims to solve the technical problem of providing a manufacturing method of the high-heat-dissipation ink, which has simple process and high production efficiency.
In order to solve the technical problems, the invention provides high-heat-dissipation ink which comprises the following preparation raw materials in parts by weight: 30-50 parts of modified epoxy glue, 15-25 parts of solvent, 10-20 parts of curing agent, 10-20 parts of filler, 0.5-3 parts of catalyst, 0.5-1 part of dispersing agent, 2-7 parts of defoaming agent and 0.1-2 parts of carbon nano tube;
the modified epoxy glue at least comprises epoxy resin, and the volume of the epoxy resin accounts for 20-50% of the volume of the modified epoxy glue;
wherein, the solvent comprises one or more of propylene glycol methyl ether acetate, ethylene glycol monobutyl ether and propylene glycol diacetate;
the filler comprises at least nano barium sulfate.
Preferably, the modified epoxy glue comprises epoxy resin and glue B;
the acid value of the B glue is lower than 115mgKOH/g, and the preparation raw materials comprise, by weight, 25-35 parts of phthalic anhydride, 65-75 parts of polyether polyol and 15-35 parts of propylene glycol methyl ether acetate.
Preferably, the solvent comprises one or more of propylene glycol methyl ether acetate, ethylene glycol monobutyl ether and propylene glycol diacetate.
Preferably, the curing agent comprises one or both of a polyether polyol and phthalic anhydride.
Preferably, the filler also comprises nano silica, and the weight of the nano barium sulfate is not less than 50% of the total weight of the filler.
Preferably, the catalyst comprises one or more of methyl benzene sulfonic acid and N, N-dimethylamino pyridine.
Preferably, the dispersant is sodium dodecyl diphenyl oxide disulfonate.
Preferably, the defoamer is a glycol siloxane.
A preparation method of the high-heat-dissipation ink comprises the following steps:
step S1, stirring the solvent for 15-20 minutes at the speed of 800-;
s2, slowly adding the filler, the dispersant and the catalyst into the stirred solvent, stirring for 5-15 minutes at the speed of 800-;
step S3, adding the modified epoxy glue into the mixed solution A, then adding the defoaming agent, and stirring for 5-10 minutes at the speed of 700 and 1000 revolutions per minute at the temperature of 40-70 ℃ under normal pressure to obtain a mixed solution B;
step S4, adding carbon nano tubes into the mixed solution B, and stirring for 5-8 minutes at the speed of 600-;
and step S5, adding a curing agent into the mixed solution C, uniformly stirring, and filtering to obtain a finished product.
Preferably, the preparation method of the modified epoxy glue comprises the following steps:
step S31, adding phthalic anhydride and polyether polyol into a reaction kettle, stirring, keeping the temperature at 100-140 ℃, keeping the temperature for 30-60min, then heating to 160-180 ℃, keeping the temperature for 4-6H, and cooling to below 100 ℃ to obtain a mixed solution B1;
and S32, adding propylene glycol encrypted acetate into the mixed solution B1 for dilution to obtain a finished modified epoxy adhesive product, wherein the acid value of the finished modified epoxy adhesive product is lower than 115 mgKOH/g.
The implementation of the invention has the following beneficial effects:
1. the high-heat-dissipation ink obtained by the proportioning is obtained by mutual reaction among various raw materials, has strong adhesive force and chemical resistance, and improves the wear resistance of the ink by adding the filler on the premise of not influencing the optical performance of the ink.
2. The ink of the invention increases the heat dissipation capability of the ink by adding the carbon nano tube, so that the high heat dissipation ink can be normally used in equipment with large heat productivity, thereby preventing heat from gathering, burning electronic components in the equipment and ensuring the reliability of the equipment.
3. According to the ink disclosed by the invention, the epoxy resin is modified, the ink is prevented from being peeled and cracked, the adhesive force of the ink is ensured, and the raw materials have good reactivity and are matched with each other, so that the ink with excellent quality is obtained.
4. According to the preparation method of the ink, various raw materials are sequentially added according to the steps of the invention, so that the raw materials react with each other to obtain a required mixture, the performances of wear resistance, corrosion resistance, optics and the like of the ink are met, the process is simple, and the production efficiency is high; the ink prepared by the method has strong heat dissipation capacity and strong adhesive force, and is particularly suitable for equipment with large heat productivity.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention will be described in further detail below.
The invention provides high-heat-dissipation printing ink which comprises the following preparation raw materials in parts by weight: 30-50 parts of modified epoxy glue, 15-25 parts of solvent, 10-20 parts of curing agent, 10-20 parts of filler, 0.5-3 parts of catalyst, 0.5-1 part of dispersing agent, 2-7 parts of defoaming agent and 0.1-2 parts of carbon nano tube;
the modified epoxy glue at least comprises epoxy resin, and the volume of the epoxy resin accounts for 20-50% of the volume of the modified epoxy glue;
wherein, the solvent comprises one or more of propylene glycol methyl ether acetate, ethylene glycol monobutyl ether and propylene glycol diacetate;
the filler comprises at least nano barium sulfate.
The modified epoxy glue at least comprises epoxy resin, and the epoxy resin has good adhesion, high strength, corrosion resistance and the like, but the epoxy resin is easy to generate larger internal stress after being cured, and the cured product has poor flexibility, brittle and hard texture and easy cracking, so the modified epoxy glue needs to be modified.
Specifically, the modified epoxy glue comprises epoxy resin and glue B, the acid value of the glue B is lower than 115mgKOH/g, and the preparation raw materials comprise, by weight, 25-35 parts of phthalic anhydride, 65-75 parts of polyether polyol and 15-35 parts of propylene glycol monomethyl ether acetate.
The solvent comprises one or more of propylene glycol methyl ether acetate, ethylene glycol monobutyl ether and propylene glycol diacetate.
The curing agent comprises one or two of polyether polyol and phthalic anhydride, and the good reactivity between the curing agent and the epoxy resin is utilized to improve the performance of the high-heat-dissipation ink.
The filler at least comprises nano barium sulfate, and the barium sulfate has good dispersibility in epoxy resin, is an aid capable of adjusting the concentration of the ink, can increase the thickness of the rubbed ink and improve the wear resistance of the rubbed ink, so that in the embodiment, when the filler also comprises other materials, the weight of the nano barium sulfate is not less than 50% of the total weight of the filler.
In order to further increase the wear resistance of the high heat dissipation ink, the filler also comprises nano silicon dioxide, because the hardness of the silicon dioxide is high, and the addition of the silicon dioxide in the ink can obviously improve the scratch resistance and the wear resistance of a coating film. However, the use of silica affects other properties of the coating film, such as reduced gloss and increased haze. Therefore, the nano-silica is selected as the raw material of the scratch resistance agent, the particle size of the nano-silica is small, on the other hand, the content of the nano-silica is controlled to be less than 50 percent of the total weight of the filler, the comprehensive performance of the nano-barium sulfate and the nano-silica is fully utilized, the optical performance and the wear resistance of the ink such as glossiness and the like are ensured, and the ink with excellent quality is obtained.
The catalyst comprises one or more of methyl benzene sulfonic acid and N, N-dimethylamino pyridine.
The dispersant is sodium dodecyl diphenyl oxide disulfonate, and has excellent dispersing, wetting and emulsifying capacities.
The defoaming agent is ethylene glycol siloxane;
the carbon nano tubes are uniformly mixed in the raw materials and used for improving the heat dissipation performance of the raw materials, wherein the content of the carbon nano tubes is 0.1-2 parts, the heat dissipation effect is poor due to too low content, the physical performance of the ink is affected due to too high content, and the production cost is high.
According to the high-heat-dissipation ink provided by the invention, the wear resistance of the ink is improved through the arrangement of the filler, the optical performance of the ink is not influenced, the epoxy resin is modified, the ink is prevented from being stripped and cracked, the adhesive force of the ink is ensured, and the raw materials have good reactivity and are matched with each other to obtain the ink with excellent quality.
Through the addition of the carbon nano tube, the heat dissipation capacity of the ink is improved, so that the high-heat-dissipation ink can be normally used in equipment with large heat productivity, heat accumulation is prevented, electronic components in the equipment are burnt out, and the reliability of the equipment is ensured.
Correspondingly, the invention also provides a preparation method of the high heat dissipation ink, which comprises the following steps:
step S1, stirring the solvent for 15-20 minutes at the speed of 800-;
s2, slowly adding the filler, the dispersant and the catalyst into the stirred solvent, stirring for 5-15 minutes at the speed of 800-;
step S3, adding the modified epoxy glue into the mixed solution A, then adding the defoaming agent, and stirring for 5-10 minutes at the speed of 700 and 1000 revolutions per minute at the temperature of 40-70 ℃ under normal pressure to obtain a mixed solution B;
the preparation method of the modified epoxy glue comprises the following steps:
step S31, adding phthalic anhydride and polyether polyol into a reaction kettle, stirring, keeping the temperature at 100-140 ℃, keeping the temperature for 30-60min, then heating to 160-180 ℃, keeping the temperature for 4-6H, and cooling to below 100 ℃ to obtain a mixed solution B1;
and S32, adding propylene glycol encrypted acetate into the mixed solution B1 for dilution to obtain a finished modified epoxy adhesive product, wherein the acid value of the finished modified epoxy adhesive product is lower than 115 mgKOH/g.
Step S4, adding carbon nano tubes into the mixed solution B, and stirring for 5-8 minutes at the speed of 600-;
and step S5, adding a curing agent into the mixed solution C, uniformly stirring, and filtering to obtain a finished product.
The high-heat-dissipation ink obtained by the proportioning is obtained by mutual reaction of various raw materials, has strong adhesive force and chemical resistance, and improves the wear resistance of the ink by adding the filler on the premise of not influencing the optical performance of the ink.
The ink disclosed by the invention has the advantages that the heat dissipation capacity of the ink is increased by adding the carbon nano tubes, so that the high-heat-dissipation ink can be normally used in equipment with large heat productivity, the heat accumulation is prevented, electronic components in the equipment are burnt out, and the reliability of the equipment is ensured.
According to the ink disclosed by the invention, the epoxy resin is modified, the ink is prevented from being peeled and cracked, the adhesive force of the ink is ensured, and the raw materials have good reactivity and are matched with each other, so that the ink with excellent quality is obtained.
According to the preparation method of the ink, various raw materials are sequentially added according to the steps of the invention, so that the raw materials react with each other to obtain a required mixture, the performances of wear resistance, corrosion resistance, optics and the like of the ink are met, the process is simple, and the production efficiency is high; the ink prepared by the method has strong heat dissipation capacity and strong adhesive force, and is particularly suitable for equipment with large heat productivity.
Example 1
The embodiment provides a high heat dissipation ink, which comprises the following preparation raw materials: 30 parts of modified epoxy glue, 15 parts of solvent, 10 parts of curing agent, 10 parts of filler, 0.5 part of catalyst, 0.5 part of dispersing agent, 2 parts of defoaming agent and 0.1 part of carbon nano tube;
the modified epoxy glue comprises epoxy resin and glue B, wherein the volume of the epoxy resin accounts for 20% of that of the modified epoxy glue;
the acid value of the B glue is 113mgKOH/g, and the preparation raw materials comprise 25 parts of phthalic anhydride, 65 parts of polyether polyol and 15 parts of propylene glycol monomethyl ether acetate;
the solvent is propylene glycol methyl ether acetate; the curing agent is polyether polyol;
the filler comprises nano barium sulfate and nano silicon dioxide, and the weight of the nano barium sulfate is 50% of the total weight of the filler.
The catalyst is methyl benzenesulfonic acid, the dispersing agent is sodium dodecyl diphenyl ether disulfonate, and the defoaming agent is ethylene glycol siloxane.
Correspondingly, the embodiment also provides a preparation method of the high heat dissipation ink, which comprises the following steps:
step S1, stirring the solvent for 15 minutes at the speed of 800 rpm at the temperature of 50 ℃ under the pressure of normal pressure to obtain the stirred solvent;
step S2, slowly adding the filler, the dispersant and the catalyst into the stirred solvent, stirring for 5 minutes at the speed of 800 rpm at the temperature of 50 ℃ under normal pressure to obtain a mixed solution A;
step S3, adding the modified epoxy glue into the mixed solution A, then adding the defoaming agent, and stirring for 5 minutes at the speed of 700 revolutions per minute and at the temperature of 40 ℃ and under the normal pressure to obtain mixed solution B;
the preparation method of the modified epoxy glue comprises the following steps:
step S31, adding phthalic anhydride and polyether polyol into a reaction kettle, stirring, keeping the temperature at 100 ℃ for 30min, then heating to 160 ℃, keeping the temperature for 4H, and cooling to below 90 ℃ to obtain a mixed solution B1;
and S32, adding propylene glycol encrypted acetate into the mixed solution B1 for dilution to obtain a finished modified epoxy adhesive product with an acid value of 113 mgKOH/g.
Step S4, adding the carbon nano tube into the mixed solution B, and stirring for 5 minutes at the speed of 600 revolutions per minute at the temperature of 30 ℃ and under the pressure of 8MPa to obtain mixed solution C;
and step S5, adding a curing agent into the mixed solution C, uniformly stirring, and filtering to obtain a finished product.
Example 2
The embodiment provides a high heat dissipation ink, which comprises the following preparation raw materials: 50 parts of modified epoxy glue, 25 parts of solvent, 20 parts of curing agent, 20 parts of filler, 3 parts of catalyst, 1 part of dispersing agent, 7 parts of defoaming agent and 2 parts of carbon nano tube;
the modified epoxy glue comprises epoxy resin and glue B, wherein the volume of the epoxy resin accounts for 50% of that of the modified epoxy glue;
the acid value of the B glue is 110mgKOH/g, and the preparation raw materials comprise 35 parts of phthalic anhydride, 75 parts of polyether polyol and 35 parts of propylene glycol methyl ether acetate;
the solvent is propylene glycol methyl ether acetate; the curing agent is polyether polyol;
the filler comprises nano barium sulfate and nano silica, and the weight of the nano barium sulfate is 60% of the total weight of the filler.
The catalyst is methyl benzenesulfonic acid, the dispersing agent is sodium dodecyl diphenyl ether disulfonate, and the defoaming agent is ethylene glycol siloxane.
Correspondingly, the embodiment also provides a preparation method of the high heat dissipation ink, which comprises the following steps:
step S1, stirring the solvent for 20 minutes at the speed of 1200 rpm, the temperature of 80 ℃ and the pressure of normal pressure to obtain the solvent which is stirred;
step S2, slowly adding the filler, the dispersant and the catalyst into the stirred solvent, stirring for 15 minutes at the speed of 1200 rpm at the temperature of 80 ℃ under normal pressure to obtain a mixed solution A;
step S3, adding the modified epoxy glue into the mixed solution A, then adding the defoaming agent, and stirring for 10 minutes at the speed of 1000 rpm, the temperature of 70 ℃ and the pressure of normal pressure to obtain mixed solution B;
the preparation method of the modified epoxy glue comprises the following steps:
step S31, adding phthalic anhydride and polyether polyol into a reaction kettle, stirring, keeping the temperature at 140 ℃ for 60min, then heating to 180 ℃, keeping the temperature for 6H, and cooling to 95 ℃ to obtain a mixed solution B1;
and S32, adding propylene glycol encrypted acetate into the mixed solution B1 for dilution to obtain a finished modified epoxy adhesive product, wherein the acid value of the finished modified epoxy adhesive product is 110 mgKOH/g.
Step S4, adding carbon nanotubes into the mixed solution B, and stirring for 8 minutes at the speed of 1000 rpm, the temperature of 70 ℃ and the pressure of 8MPa to obtain mixed solution C;
and step S5, adding a curing agent into the mixed solution C, uniformly stirring, and filtering to obtain a finished product.
Example 3
The embodiment provides a high heat dissipation ink, which comprises the following preparation raw materials: 40 parts of modified epoxy glue, 20 parts of solvent, 15 parts of curing agent, 15 parts of filler, 2 parts of catalyst, 0.8 part of dispersing agent, 5 parts of defoaming agent and 1 part of carbon nano tube;
the modified epoxy glue comprises epoxy resin and glue B, wherein the volume of the epoxy resin accounts for 30% of that of the modified epoxy glue;
the acid value of the B glue is 108mgKOH/g, and the preparation raw materials comprise 30 parts of phthalic anhydride, 70 parts of polyether polyol and 25 parts of propylene glycol monomethyl ether acetate;
the solvent is propylene glycol methyl ether acetate; the curing agent is polyether polyol;
the filler comprises nano barium sulfate and nano silicon dioxide, and the weight of the nano barium sulfate is 65% of the total weight of the filler.
The catalyst is methyl benzenesulfonic acid, the dispersing agent is sodium dodecyl diphenyl ether disulfonate, and the defoaming agent is ethylene glycol siloxane.
Correspondingly, the embodiment also provides a preparation method of the high heat dissipation ink, which comprises the following steps:
step S1, stirring the solvent for 18 minutes at the speed of 1000 rpm, the temperature of 70 ℃ and the pressure of normal pressure to obtain the solvent which is stirred;
step S2, slowly adding the filler, the dispersant and the catalyst into the stirred solvent, stirring for 18 minutes at the speed of 1000 rpm at the temperature of 60 ℃ under normal pressure to obtain a mixed solution A;
step S3, adding the modified epoxy glue into the mixed solution A, then adding the defoaming agent, and stirring for 10 minutes at the speed of 900 rpm at the temperature of 50 ℃ under normal pressure to obtain mixed solution B;
the preparation method of the modified epoxy glue comprises the following steps:
step S31, adding phthalic anhydride and polyether polyol into a reaction kettle, stirring, keeping the temperature at 120 ℃ for 40min, then heating to 170 ℃, keeping the temperature for 5H, and cooling to 85 ℃ to obtain a mixed solution B1;
and S32, adding propylene glycol encrypted acetate into the mixed solution B1 for dilution to obtain a finished modified epoxy adhesive product, wherein the acid value of the finished modified epoxy adhesive product is 108 mgKOH/g.
Step S4, adding the carbon nano tube into the mixed solution B, and stirring for 7 minutes at the speed of 800 rpm, the temperature of 50 ℃ and the pressure of 8MPa to obtain mixed solution C;
and step S5, adding a curing agent into the mixed solution C, uniformly stirring, and filtering to obtain a finished product.
Comparative example 1
This example is substantially the same as the above examples, except that a conventional epoxy resin is used, and specifically, a high heat dissipation ink is provided, which is prepared from the following raw materials: 40 parts of modified epoxy glue, 20 parts of solvent, 15 parts of curing agent, 15 parts of filler, 2 parts of catalyst, 0.8 part of dispersing agent, 5 parts of defoaming agent and 1 part of carbon nano tube;
wherein the modified epoxy glue is epoxy resin;
the solvent is propylene glycol methyl ether acetate; the curing agent is polyether polyol;
the filler comprises nano barium sulfate and nano silicon dioxide, and the weight of the nano barium sulfate is 65% of the total weight of the filler.
The catalyst is methyl benzenesulfonic acid, the dispersing agent is sodium dodecyl diphenyl ether disulfonate, and the defoaming agent is ethylene glycol siloxane.
Correspondingly, the embodiment also provides a preparation method of the high heat dissipation ink, which comprises the following steps:
step S1, stirring the solvent for 18 minutes at the speed of 1000 rpm, the temperature of 70 ℃ and the pressure of normal pressure to obtain the solvent which is stirred;
step S2, slowly adding the filler, the dispersant and the catalyst into the stirred solvent, stirring for 18 minutes at the speed of 1000 rpm at the temperature of 60 ℃ under normal pressure to obtain a mixed solution A;
step S3, adding the modified epoxy glue into the mixed solution A, then adding the defoaming agent, and stirring for 10 minutes at the speed of 900 rpm at the temperature of 50 ℃ under normal pressure to obtain mixed solution B;
step S4, adding the carbon nano tube into the mixed solution B, and stirring for 7 minutes at the speed of 800 rpm, the temperature of 50 ℃ and the pressure of 8MPa to obtain mixed solution C;
and step S5, adding a curing agent into the mixed solution C, uniformly stirring, and filtering to obtain a finished product.
Comparative example 2
This example is substantially the same as the above examples, except that no carbon nanotubes are added to the raw materials, specifically, a high heat dissipation ink is provided, which comprises the following raw materials: 40 parts of modified epoxy glue, 20 parts of solvent, 15 parts of curing agent, 15 parts of filler, 2 parts of catalyst, 0.8 part of dispersing agent and 5 parts of defoaming agent;
the modified epoxy glue comprises epoxy resin and glue B, wherein the volume of the epoxy resin accounts for 30% of that of the modified epoxy glue;
the acid value of the B glue is 108mgKOH/g, and the preparation raw materials comprise 30 parts of phthalic anhydride, 70 parts of polyether polyol and 25 parts of propylene glycol monomethyl ether acetate;
the solvent is propylene glycol methyl ether acetate; the curing agent is polyether polyol;
the filler comprises nano barium sulfate and nano silicon dioxide, and the weight of the nano barium sulfate is 65% of the total weight of the filler.
The catalyst is methyl benzenesulfonic acid, the dispersing agent is sodium dodecyl diphenyl ether disulfonate, and the defoaming agent is ethylene glycol siloxane.
Correspondingly, the embodiment also provides a preparation method of the high heat dissipation ink, which comprises the following steps:
step S1, stirring the solvent for 18 minutes at the speed of 1000 rpm, the temperature of 70 ℃ and the pressure of normal pressure to obtain the solvent which is stirred;
step S2, slowly adding the filler, the dispersant and the catalyst into the stirred solvent, stirring for 18 minutes at the speed of 1000 rpm at the temperature of 60 ℃ under normal pressure to obtain a mixed solution A;
step S3, adding the modified epoxy glue into the mixed solution A, then adding the defoaming agent, and stirring for 10 minutes at the speed of 900 rpm at the temperature of 50 ℃ under normal pressure to obtain mixed solution B;
the preparation method of the modified epoxy glue comprises the following steps:
step S31, adding phthalic anhydride and polyether polyol into a reaction kettle, stirring, keeping the temperature at 120 ℃ for 40min, then heating to 170 ℃, keeping the temperature for 5H, and cooling to 85 ℃ to obtain a mixed solution B1;
and S32, adding propylene glycol encrypted acetate into the mixed solution B1 for dilution to obtain a finished modified epoxy adhesive product, wherein the acid value of the finished modified epoxy adhesive product is 108 mgKOH/g.
And step S5, adding a curing agent into the mixed liquid B, uniformly stirring, and filtering to obtain a finished product.
Comparative example 3
The difference between this embodiment and the above embodiments is that, in this embodiment, no nano silicon dioxide is added, and this embodiment provides a high heat dissipation ink, which includes the following raw materials: 40 parts of modified epoxy glue, 20 parts of solvent, 15 parts of curing agent, 15 parts of filler, 2 parts of catalyst, 0.8 part of dispersing agent, 5 parts of defoaming agent and 1 part of carbon nano tube;
the modified epoxy glue comprises epoxy resin and glue B, wherein the volume of the epoxy resin accounts for 30% of that of the modified epoxy glue;
the acid value of the B glue is 108mgKOH/g, and the preparation raw materials comprise 30 parts of phthalic anhydride, 70 parts of polyether polyol and 25 parts of propylene glycol monomethyl ether acetate;
the solvent is propylene glycol methyl ether acetate; the curing agent is polyether polyol;
the filler comprises nano barium sulfate. The catalyst is methyl benzene sulfonic acid, the dispersing agent is sodium dodecyl diphenyl ether disulfonate, and the defoaming agent is ethylene glycol siloxane.
Correspondingly, the embodiment also provides a preparation method of the high heat dissipation ink, which comprises the following steps:
step S1, stirring the solvent for 18 minutes at the speed of 1000 rpm, the temperature of 70 ℃ and the pressure of normal pressure to obtain the solvent which is stirred;
step S2, slowly adding the filler, the dispersant and the catalyst into the stirred solvent, stirring for 18 minutes at the speed of 1000 rpm at the temperature of 60 ℃ under normal pressure to obtain a mixed solution A;
step S3, adding the modified epoxy glue into the mixed solution A, then adding the defoaming agent, and stirring for 10 minutes at the speed of 900 rpm at the temperature of 50 ℃ under normal pressure to obtain mixed solution B;
the preparation method of the modified epoxy glue comprises the following steps:
step S31, adding phthalic anhydride and polyether polyol into a reaction kettle, stirring, keeping the temperature at 120 ℃ for 40min, then heating to 170 ℃, keeping the temperature for 5H, and cooling to 85 ℃ to obtain a mixed solution B1;
and S32, adding propylene glycol encrypted acetate into the mixed solution B1 for dilution to obtain a finished modified epoxy adhesive product, wherein the acid value of the finished modified epoxy adhesive product is 108 mgKOH/g.
Step S4, adding the carbon nano tube into the mixed solution B, and stirring for 7 minutes at the speed of 800 rpm, the temperature of 50 ℃ and the pressure of 8MPa to obtain mixed solution C;
and step S5, adding a curing agent into the mixed solution C, uniformly stirring, and filtering to obtain a finished product.
The ink obtained by the method is coated on a PCB (printed Circuit Board), and is dried and tested, and the high-heat-dissipation ink prepared by the method and the formula has the following properties:
the adhesive force in the upper table is used for pulling the ink on the PCB by using an adhesive tape method, and whether the ink is peeled off or not is tested, and the ink is unqualified if the ink is peeled off, and is not qualified if the ink is not peeled off.
The surface temperature of the upper table is obtained by measuring the surface temperature of the display screen after the PCB is applied to the display screen and works for one hour.
While the invention has been described in connection with what is presently considered to be the most practical and preferred embodiment, it is to be understood that the invention is not to be limited to the disclosed embodiment, but on the contrary, is intended to cover various modifications and equivalent arrangements included within the spirit and scope of the appended claims.
Claims (10)
1. The high-heat-dissipation printing ink is characterized by comprising the following preparation raw materials in parts by weight: 30-50 parts of modified epoxy glue, 15-25 parts of solvent, 10-20 parts of curing agent, 10-20 parts of filler, 0.5-3 parts of catalyst, 0.5-1 part of dispersing agent, 2-7 parts of defoaming agent and 0.1-2 parts of carbon nano tube;
the modified epoxy glue at least comprises epoxy resin, and the volume of the epoxy resin accounts for 20-50% of the volume of the modified epoxy glue;
wherein, the solvent comprises one or more of propylene glycol methyl ether acetate, ethylene glycol monobutyl ether and propylene glycol diacetate;
the filler comprises at least nano barium sulfate.
2. The high heat dissipation ink of claim 1, wherein the modified epoxy glue comprises an epoxy resin and a glue B;
the acid value of the B glue is lower than 115mgKOH/g, and the preparation raw materials comprise, by weight, 25-35 parts of phthalic anhydride, 65-75 parts of polyether polyol and 15-35 parts of propylene glycol methyl ether acetate.
3. The high heat dissipation ink according to claim 1, wherein the solvent includes one or more of propylene glycol methyl ether acetate, ethylene glycol monobutyl ether, and propylene glycol diacetate.
4. The high heat dissipation ink of claim 1, wherein the curing agent comprises one or both of a polyether polyol and phthalic anhydride.
5. The high thermal dissipation ink of claim 1, wherein the filler further comprises nano silica, and the weight of the nano barium sulfate is not less than 50% of the total weight of the filler.
6. The high heat dissipation ink of claim 1, wherein the catalyst comprises one or more of methyl benzene sulfonic acid and N, N-dimethylaminopyridine.
7. The high heat dissipation ink of claim 1, wherein the dispersant is sodium dodecyl diphenyl oxide disulfonate.
8. The high heat dissipation ink of claim 1, wherein the antifoaming agent is ethylene glycol siloxane.
9. A preparation method of the high heat dissipation ink of any one of claims 1 to 8 is characterized by comprising the following steps:
step S1, stirring the solvent for 15-20 minutes at the speed of 800-;
s2, slowly adding the filler, the dispersant and the catalyst into the stirred solvent, stirring for 5-15 minutes at the speed of 800-;
step S3, adding the modified epoxy glue into the mixed solution A, then adding the defoaming agent, and stirring for 5-10 minutes at the speed of 700 and 1000 revolutions per minute at the temperature of 40-70 ℃ under normal pressure to obtain a mixed solution B;
step S4, adding carbon nano tubes into the mixed solution B, and stirring for 5-8 minutes at the speed of 600-;
and step S5, adding a curing agent into the mixed solution C, uniformly stirring, and filtering to obtain a finished product.
10. The method of claim 9, wherein the modified epoxy glue is prepared by the steps of:
step S31, adding phthalic anhydride and polyether polyol into a reaction kettle, stirring, keeping the temperature at 100-140 ℃, keeping the temperature for 30-60min, then heating to 160-180 ℃, keeping the temperature for 4-6H, and cooling to below 100 ℃ to obtain a mixed solution B1;
and S32, adding propylene glycol encrypted acetate into the mixed solution B1 for dilution to obtain a finished modified epoxy adhesive product, wherein the acid value of the finished modified epoxy adhesive product is lower than 115 mgKOH/g.
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