CN111500048A - Heat-conducting connecting foam and preparation method thereof - Google Patents
Heat-conducting connecting foam and preparation method thereof Download PDFInfo
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- CN111500048A CN111500048A CN202010386345.0A CN202010386345A CN111500048A CN 111500048 A CN111500048 A CN 111500048A CN 202010386345 A CN202010386345 A CN 202010386345A CN 111500048 A CN111500048 A CN 111500048A
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Abstract
The invention relates to heat-conducting connecting foam and a preparation method thereof, wherein the foam comprises the following raw material components in parts by weight: 8-10 parts of polycarbonate diol, 12-15 parts of xylylene diisocyanate, 4-9 parts of vinyl polysiloxane, 2-4 parts of 2-hydroxypropionic acid, 0.6-1.0 part of graphene oxide, 20-30 parts of pentaerythritol, 15-20 parts of polyethyleneimine, 0.5-1 part of sodium dodecyl sulfate, 1-3 parts of N-phenyl-2-naphthylamine, 0.1-0.4 part of guar gum hydroxypropyl trimethyl ammonium chloride, 3-8 parts of a foaming agent, 2-3 parts of a curing agent and 1-1.5 parts of a flame retardant. The heat-conducting connecting foam provided by the invention has the advantages of good heat conductivity, high foaming rate in the foam, uniform and fine foam holes, stable performance in all aspects, excellent compression resilience, flame retardance, waterproofness and structural stability, low production cost and wide application prospect.
Description
Technical Field
The invention relates to the technical field of foam, in particular to heat-conducting connecting foam and a preparation method thereof.
Background
The foam is made of foamed plastic particles, and is divided into PU foam, antistatic foam, conductive foam, EPE, antistatic EPE, PORON, CR, EVA, bridging PE, SBR, EPDM, etc. The foam has the characteristics of good elasticity, light weight, quick pressure-sensitive fixation, convenient use, free bending, ultrathin volume, reliable performance and the like.
As the electronic information industry becomes the major driving industry for the growth of GDP, the market of electronic products, such as notebook computers, large-scale liquid crystal displays, high-power supplies, etc., is getting bigger and bigger, and for these electronic products, good heat dissipation is an important factor for ensuring the normal and continuous operation thereof; it is shown that for every 2 ℃ rise of the temperature of the electronic component, the reliability is reduced by 10%, and the service life at 50 ℃ is only 1/6 at 25 ℃, the improvement of the heat conduction performance is generally accompanied with the optimization of the heat dissipation performance, so that the heat conduction gap interface material foam product is more and more concerned. Although several foam materials with heat conduction effect have appeared at present, the defects of low heat conduction coefficient, poor temperature uniformity, high production cost and the like still exist. Therefore, a further solution is necessary to provide a heat-conducting connection foam with high heat conductivity and good temperature uniformity.
Disclosure of Invention
Aiming at the defects in the prior art, the invention aims to provide heat-conducting connection foam and a preparation method thereof so as to improve the heat conductivity coefficient and the temperature uniformity of the foam, and improve the compression resilience, the flame retardance, the waterproofness and the like of the foam.
In order to achieve the purpose, the technical scheme provided by the invention is as follows:
in a first aspect, the invention provides heat-conducting connecting foam, which comprises the following raw material components in parts by weight: 8-10 parts of polycarbonate diol, 12-15 parts of xylylene diisocyanate, 4-9 parts of vinyl polysiloxane, 2-4 parts of 2-hydroxypropionic acid, 0.6-1.0 part of graphene oxide, 20-30 parts of pentaerythritol, 15-20 parts of polyethyleneimine, 0.5-1 part of sodium dodecyl sulfate, 1-3 parts of N-phenyl-2-naphthylamine, 0.1-0.4 part of guar gum hydroxypropyl trimethyl ammonium chloride, 3-8 parts of a foaming agent, 2-3 parts of a curing agent and 1-1.5 parts of a flame retardant.
Preferably, the heat-conducting connecting foam provided by the invention further comprises the following raw material components in parts by weight: 12-15 parts of ethylene-vinyl acetate copolymer, 10-16 parts of modified carbon fiber, 1-2 parts of coniferyl alcohol, 1-1.5 parts of cashew nut oil and 5-7 parts of phenolic resin.
Further preferably, the heat-conducting connecting foam provided by the invention comprises the following raw material components in parts by weight: 9 parts of polycarbonate diol, 13 parts of xylylene diisocyanate, 6 parts of vinyl polysiloxane, 3 parts of 2-hydroxypropionic acid, 0.8 part of graphene oxide, 25 parts of pentaerythritol, 17 parts of polyethyleneimine, 0.8 part of sodium dodecyl sulfate, 2 parts of N-phenyl-2-naphthylamine, 0.3 part of guar gum hydroxypropyl trimethyl ammonium chloride, 5 parts of a foaming agent, 2.5 parts of a curing agent, 1.2 parts of a flame retardant, 14 parts of an ethylene-vinyl acetate copolymer, 13 parts of modified carbon fibers, 1.6 parts of coniferyl alcohol, 1.3 parts of cashew nut oil and 6 parts of phenolic resin.
The polycarbonate diol used in the invention preferably has a hydroxyl value in the range of 150mgKOH/g-500mgKOH/g and a number average molecular weight in the range of 200-1800, and is further preferably polycarbonate diol (PCD L-1000), the vinyl polysiloxane used in the invention is one or a combination of several of vinyl-terminated polydimethylsiloxane, vinyl-terminated polymethylvinylsiloxane and polyvinyl bisphenylpolysiloxane, preferably the vinyl-terminated polydimethylsiloxane with a vinyl content of 0.3%, the foaming agent used in the invention is dichloromethane and/or fluorotrichloromethane, the curing agent used in the invention is formic acid and/or acetic acid, the flame retardant used in the invention is one or more selected from aluminum magnesium flame retardants, nitrogen flame retardants, organosilicon flame retardants and zinc borate flame retardants, and the mass content of vinyl acetate in the ethylene-vinyl acetate copolymer (EVA) used in the invention is preferably 33%, and the melt index at 190 ℃ is preferably 43g/10 min.
Preferably, the preparation method of the raw material component modified carbon fiber of the heat-conducting connecting foam provided by the invention comprises the following steps: mixing carbon fiber and p-aminobenzoic acid in a ratio of 1: (40-50), adding a sodium hydroxide solution at the temperature of 190-210 ℃ for reaction for 45-60h, adding acetic acid to adjust the pH value to 4-4.5, standing for 80-100h, and drying to obtain the modified carbon fiber.
Preferably, the preparation method of the cashew nut oil as the raw material component of the heat-conducting connecting foam provided by the invention comprises the following steps: mixing cashew nut kernels and an ethanol water solution in a proportion of 100: (40-50), and heating at 80-95 ℃ for 60-70min to obtain a cashew nut mixture; crushing cashew shell to a particle size of less than 0.2mm, and then drying until the water content is not higher than 3% to obtain cashew shell powder; uniformly mixing the cashew nut mixture and cashew nut shell powder, then squeezing at the temperature of 45-50 ℃ by adopting a double-screw oil press, filtering the obtained crude oil, and collecting filtrate to obtain the cashew nut oil.
Further preferably, in the preparation method of the cashew nut oil as the raw material component of the heat-conducting connecting foam, the volume fraction of ethanol in the ethanol water solution is 65-75%; the mass ratio of the cashew nut mixture to the cashew nut shell powder is 1: (2-3).
In a second aspect, the invention provides a preparation method of heat-conducting connecting foam, which comprises the following steps: carrying out oscillation dispersion on polycarbonate diol, xylylene diisocyanate, vinyl polysiloxane, 2-hydroxy propionic acid and graphene oxide for 2-3h under the ultrasonic wave with the power of 400-500W to form a blend; adding the blend into a stirrer, adjusting the pH value to 7.5-7.8 under the condition that the stirring speed is 100-120r/min, then heating to 210 ℃ at the heating rate of 2-4 ℃/min, and preserving the heat for 40-50 min; then adding other residual raw material components, adjusting the pH value to 4.5-5.5 under the condition that the stirring speed is 130-plus-150 r/min, cooling to 140-plus-145 ℃ at the cooling speed of 0.5-1 ℃/min, then preserving the temperature for 20-30min, then foaming for 10-12min in a foaming furnace with the frequency of 2000-plus-2200 MHz and the power of 4-5kW, and then drying for 4-5h in an oven to obtain the heat-conducting connecting foam.
The invention also provides another preparation method of the heat-conducting connecting foam, which comprises the following steps: the method comprises the following steps: uniformly mixing modified carbon fiber, cashew nut oil and phenolic resin, adjusting the pH value to 8.0-8.4, then heating at 180 ℃ for 40-50min, adding polycarbonate diol, xylylene diisocyanate, vinyl polysiloxane, 2-hydroxypropionic acid and graphene oxide into the obtained mixture, and oscillating and dispersing for 2-3h under the ultrasonic wave with the power of 400 DEG and 500W to form a blend; step two, adding the blend into a stirrer, adjusting the pH value to 7.5-7.8, then heating to 210 ℃, adding the ethylene-vinyl acetate copolymer and coniferyl alcohol, and keeping the temperature for 40-50 min; step three, adding other residual raw material components into the product obtained in the step two, adjusting the pH value to 4.5-5.5, then cooling to 140-; and step four, foaming the product obtained in the step three in a foaming furnace with the frequency of 2000-2200MHz and the power of 4-5kW for 10-12min, and then drying in an oven for 4-5h to obtain the heat-conducting connecting foam.
Preferably, in the second step of the preparation method of the heat-conducting connecting foam provided by the invention, the stirring speed is 100-120r/min, and the temperature rise speed of temperature rise is 2-4 ℃/min.
Preferably, in the third step of the preparation method of the heat-conducting connecting foam provided by the invention, the stirring speed is 130-150r/min, and the cooling speed of cooling is 0.5-1 ℃/min.
The technical scheme provided by the invention has the following beneficial effects: (1) the heat-conducting connecting foam provided by the invention has the advantages that under the synergistic effect of the components, the heat-conducting connecting foam is high in heat conductivity coefficient, good in temperature uniformity, high in foaming rate inside the foam, uniform and fine in foam holes, stable in performance in all aspects, and excellent in compression resilience, flame retardance, waterproofness and structural stability; (2) on the basis of basic raw materials, the ethylene-vinyl acetate copolymer, the modified carbon fiber, the coniferyl alcohol, the cashew nut oil and the phenolic resin are adopted, so that the comprehensive performance of the prepared heat-conducting connecting foam is remarkably improved, and particularly, the natural plant product cashew nut oil is creatively used as a raw material component, so that the heat-conducting connecting foam is good in effect, environment-friendly and obvious in reinforcing effect on the foam; (3) according to the heat-conducting connecting foam provided by the invention, through a specific process, including a specific temperature rise program, a specific pH value, a specific temperature drop program, a specific charging sequence and the like in each step, the heat-conducting performance of the prepared heat-conducting connecting foam is obviously improved, and other performances are maintained to be stable and even better; and the preparation method is simple, the production cost is low, and the application prospect is good.
Additional aspects and advantages of the invention will be set forth in part in the description which follows and, in part, will be obvious from the description, or may be learned by practice of the invention.
Detailed Description
The technical solution of the present invention will be clearly and completely described below with reference to the embodiments of the present invention. The following examples are only for illustrating the technical solutions of the present invention more clearly, and therefore are only examples, and the protection scope of the present invention is not limited thereby. The experimental procedures in the following examples are conventional unless otherwise specified. The test materials used in the following examples were purchased from a conventional reagent store unless otherwise specified. In the quantitative tests in the following examples, three replicates were set, and the data are the mean or the mean ± standard deviation of the three replicates.
The raw material components for preparing the heat-conducting connecting foam are proportioned according to parts by weight, and can be increased or reduced according to corresponding proportions during production, for example, the weight can be increased or reduced by taking kilogram or ton as a unit in large-scale production and taking gram as a unit in small-scale production, but the mass proportion of the components is not changed.
The invention provides heat-conducting connecting foam which comprises the following raw material components in parts by weight: 8-10 parts of polycarbonate diol, 12-15 parts of xylylene diisocyanate, 4-9 parts of vinyl polysiloxane, 2-4 parts of 2-hydroxypropionic acid, 0.6-1.0 part of graphene oxide, 20-30 parts of pentaerythritol, 15-20 parts of polyethyleneimine, 0.5-1 part of sodium dodecyl sulfate, 1-3 parts of N-phenyl-2-naphthylamine, 0.1-0.4 part of guar gum hydroxypropyl trimethyl ammonium chloride, 3-8 parts of a foaming agent, 2-3 parts of a curing agent and 1-1.5 parts of a flame retardant.
In addition, the invention also provides a preparation method of the heat-conducting connecting foam, which comprises the following steps: carrying out oscillation dispersion on polycarbonate diol, xylylene diisocyanate, vinyl polysiloxane, 2-hydroxy propionic acid and graphene oxide for 2-3h under the ultrasonic wave with the power of 400-500W to form a blend; adding the blend into a stirrer, adjusting the pH value to 7.5-7.8 under the condition that the stirring speed is 100-120r/min, then heating to 210 ℃ at the heating rate of 2-4 ℃/min, and preserving the heat for 40-50 min; then adding other residual raw material components, adjusting the pH value to 4.5-5.5 under the condition that the stirring speed is 130-plus-150 r/min, cooling to 140-plus-145 ℃ at the cooling speed of 0.5-1 ℃/min, then preserving the temperature for 20-30min, then foaming for 10-12min in a foaming furnace with the frequency of 2000-plus-2200 MHz and the power of 4-5kW, and then drying for 4-5h in an oven to obtain the heat-conducting connecting foam.
In a further embodiment of the present invention, the raw material composition of the heat-conducting connecting foam further comprises: 12-15 parts of ethylene-vinyl acetate copolymer, 10-16 parts of modified carbon fiber, 1-2 parts of coniferyl alcohol, 1-1.5 parts of cashew nut oil and 5-7 parts of phenolic resin;
the preparation method of the modified carbon fiber comprises the following steps: mixing carbon fiber and p-aminobenzoic acid in a ratio of 1: (40-50), adding a sodium hydroxide solution at the temperature of 190-210 ℃ for reaction for 45-60h, adding acetic acid to adjust the pH value to 4-4.5, standing for 80-100h, and drying to obtain the modified carbon fiber.
The preparation method of the cashew nut oil comprises the following steps: mixing cashew nut kernels and ethanol water solution with the ethanol volume fraction of 65% -75% in a proportion of 100: (40-50), and heating at 80-95 ℃ for 60-70min to obtain a cashew nut mixture; crushing cashew shell to a particle size of less than 0.2mm, and then drying until the water content is not higher than 3% to obtain cashew shell powder; mixing cashew nut mixture and cashew shell powder in a ratio of 1: and (2) uniformly mixing the components in the mass ratio, then squeezing the mixture at the temperature of 45-50 ℃ by adopting a double-screw oil press, filtering the obtained crude oil, and collecting filtrate to obtain the cashew nut oil.
In addition, the invention also provides a preparation method of the heat-conducting connecting foam, which comprises the following steps:
the method comprises the following steps: uniformly mixing modified carbon fiber, cashew nut oil and phenolic resin, adjusting the pH value to 8.0-8.4, then heating at 180 ℃ for 40-50min, adding polycarbonate diol, xylylene diisocyanate, vinyl polysiloxane, 2-hydroxypropionic acid and graphene oxide into the obtained mixture, and oscillating and dispersing for 2-3h under the ultrasonic wave with the power of 400 DEG and 500W to form a blend;
step two, adding the blend into a stirrer, adjusting the pH value to 7.5-7.8 under the condition that the stirring speed is 100-120r/min, then heating to 210 ℃ at the heating speed of 2-4 ℃/min, adding the ethylene-vinyl acetate copolymer and coniferyl alcohol, and keeping the temperature for 40-50 min;
step three, adding other residual raw material components into the product obtained in the step two, adjusting the pH value to 4.5-5.5 under the condition that the stirring speed is 130-150r/min, then cooling to 140-145 ℃ at the cooling speed of 0.5-1 ℃/min, and then preserving heat for 20-30 min;
and step four, foaming the product obtained in the step three in a foaming furnace with the frequency of 2000-2200MHz and the power of 4-5kW for 10-12min, and then drying in an oven for 4-5h to obtain the heat-conducting connecting foam.
The following will further explain the heat-conducting connecting foam and the preparation method thereof provided by the invention by combining with specific embodiments.
Example 1
The embodiment provides a heat conduction connection foam, and the raw material composition includes by weight: 8 parts of polycarbonate diol, 15 parts of xylylene diisocyanate, 4 parts of vinyl polysiloxane, 4 parts of 2-hydroxypropionic acid, 0.6 part of graphene oxide, 30 parts of pentaerythritol, 15 parts of polyethyleneimine, 1 part of sodium dodecyl sulfate, 1 part of N-phenyl-2-naphthylamine, 0.4 part of guar gum hydroxypropyl trimethyl ammonium chloride, 3 parts of foaming agent dichloromethane, 3 parts of curing agent acetic acid and 1 part of flame retardant zinc borate.
According to the raw materials, the preparation method provided by the invention is adopted to prepare the heat-conducting connecting foam:
oscillating and dispersing polycarbonate diol, xylylene diisocyanate, vinyl polysiloxane, 2-hydroxypropionic acid and graphene oxide for 2 hours under the ultrasonic wave with the power of 400W to form a blend; adding the blend into a stirrer, adjusting the pH value to 7.5 under the condition that the stirring speed is 100r/min, then heating to 210 ℃ at the heating rate of 2 ℃/min, and preserving the heat for 40 min; and then adding other residual raw material components, adjusting the pH value to 4.5 under the condition that the stirring speed is 130r/min, cooling to 140 ℃ at the cooling speed of 0.5 ℃/min, preserving the temperature for 20min, foaming for 10min in a foaming furnace with the frequency of 2000MHz and the power of 4kW, and drying for 4h in an oven to obtain the heat-conducting connecting foam.
Example 2
The embodiment provides a heat conduction connection foam, and the raw material composition includes by weight: 10 parts of polycarbonate diol, 12 parts of xylylene diisocyanate, 9 parts of vinyl polysiloxane, 2 parts of 2-hydroxypropionic acid, 1.0 part of graphene oxide, 20 parts of pentaerythritol, 20 parts of polyethyleneimine, 0.5 part of sodium dodecyl sulfate, 3 parts of N-phenyl-2-naphthylamine, 0.1 part of guar gum hydroxypropyl trimethyl ammonium chloride, 8 parts of foaming agent dichloromethane, 2 parts of curing agent acetic acid and 1.5 parts of flame retardant zinc borate.
According to the raw materials, the preparation method provided by the invention is adopted to prepare the heat-conducting connecting foam:
oscillating and dispersing polycarbonate diol, xylylene diisocyanate, vinyl polysiloxane, 2-hydroxypropionic acid and graphene oxide for 3 hours under the ultrasonic wave with the power of 500W to form a blend; adding the blend into a stirrer, adjusting the pH value to 7.8 under the condition that the stirring speed is 120r/min, then heating to 210 ℃ at the heating rate of 4 ℃/min, and preserving the heat for 50 min; and then adding other residual raw material components, adjusting the pH value to 5.5 under the condition that the stirring speed is 150r/min, cooling to 145 ℃ at the cooling speed of 1 ℃/min, preserving the temperature for 30min, foaming for 12min in a foaming furnace with the frequency of 2200MHz and the power of 5kW, and drying for 5h in an oven to obtain the heat-conducting connecting foam.
Example 3
The embodiment provides a heat conduction connection foam, and the raw material composition includes by weight: 9 parts of polycarbonate diol, 13 parts of xylylene diisocyanate, 6 parts of vinyl polysiloxane, 3 parts of 2-hydroxypropionic acid, 0.8 part of graphene oxide, 25 parts of pentaerythritol, 17 parts of polyethyleneimine, 0.8 part of sodium dodecyl sulfate, 2 parts of N-phenyl-2-naphthylamine, 0.3 part of guar gum hydroxypropyl trimethyl ammonium chloride, 5 parts of foaming agent dichloromethane, 2.5 parts of curing agent acetic acid and 1.2 parts of flame retardant zinc borate.
According to the raw materials, the preparation method provided by the invention is adopted to prepare the heat-conducting connecting foam:
oscillating and dispersing polycarbonate diol, xylylene diisocyanate, vinyl polysiloxane, 2-hydroxypropionic acid and graphene oxide for 2.5 hours under ultrasonic waves with power of 450W to form a blend; adding the blend into a stirrer, adjusting the pH value to 7.6 under the condition that the stirring speed is 110r/min, then heating to 210 ℃ at the heating rate of 3 ℃/min, and preserving the heat for 45 min; and then adding other residual raw material components, adjusting the pH value to 5.0 under the condition that the stirring speed is 140r/min, cooling to 142 ℃ at the cooling speed of 0.8 ℃/min, preserving the temperature for 25min, foaming for 11min in a foaming furnace with the frequency of 2100MHz and the power of 4.5kW, and drying for 4.5h in an oven to obtain the heat-conducting connecting foam.
Example 4
The embodiment provides a heat conduction connection foam, and the raw material composition includes by weight: 8 parts of polycarbonate diol, 15 parts of xylylene diisocyanate, 4 parts of vinyl polysiloxane, 4 parts of 2-hydroxypropionic acid, 0.6 part of graphene oxide, 30 parts of pentaerythritol, 15 parts of polyethyleneimine, 1 part of sodium dodecyl sulfate, 1 part of N-phenyl-2-naphthylamine, 0.4 part of guar hydroxypropyl trimethyl ammonium chloride, 3 parts of foaming agent dichloromethane, 3 parts of curing agent acetic acid, 1 part of flame retardant zinc borate, 12 parts of ethylene-vinyl acetate copolymer, 16 parts of modified carbon fiber, 1 part of coniferyl alcohol, 1.5 parts of cashew nut oil and 5 parts of phenolic resin.
According to the raw materials, the preparation method provided by the invention is adopted to prepare the heat-conducting connecting foam:
the method comprises the following steps: uniformly mixing modified carbon fibers, cashew nut oil and phenolic resin, adjusting the pH value to 8.0, then heating at 160 ℃ for 40min, adding polycarbonate diol, xylylene diisocyanate, vinyl polysiloxane, 2-hydroxypropionic acid and graphene oxide into the obtained mixture, and oscillating and dispersing for 2h under the ultrasonic wave with the power of 400W to form a blend;
step two, adding the blend into a stirrer, adjusting the pH value to 7.5 under the condition that the stirring speed is 100r/min, then heating to 210 ℃ at the heating rate of 2 ℃/min, adding the ethylene-vinyl acetate copolymer and coniferyl alcohol, and keeping the temperature for 40 min;
step three, adding other residual raw material components into the product obtained in the step two, adjusting the pH value to 4.5 under the condition that the stirring speed is 130r/min, then cooling to 140 ℃ at the cooling speed of 0.5 ℃/min, and then preserving heat for 20 min;
and step four, foaming the product obtained in the step three in a foaming furnace with the frequency of 2000MHz and the power of 4kW for 10min, and then drying in an oven for 4h to obtain the heat-conducting connecting foam.
Example 5
The embodiment provides a heat conduction connection foam, and the raw material composition includes by weight: 10 parts of polycarbonate diol, 12 parts of xylylene diisocyanate, 9 parts of vinyl polysiloxane, 2 parts of 2-hydroxypropionic acid, 1.0 part of graphene oxide, 20 parts of pentaerythritol, 20 parts of polyethyleneimine, 0.5 part of sodium dodecyl sulfate, 3 parts of N-phenyl-2-naphthylamine, 0.1 part of guar hydroxypropyl trimethyl ammonium chloride, 8 parts of foaming agent dichloromethane, 2 parts of curing agent acetic acid, 1.5 parts of flame retardant zinc borate, 15 parts of ethylene-vinyl acetate copolymer, 10 parts of modified carbon fiber, 2 parts of coniferyl alcohol, 1 part of cashew nut oil and 7 parts of phenolic resin.
According to the raw materials, the preparation method provided by the invention is adopted to prepare the heat-conducting connecting foam:
the method comprises the following steps: uniformly mixing modified carbon fibers, cashew nut oil and phenolic resin, adjusting the pH value to 8.4, heating at 180 ℃ for 50min, adding polycarbonate diol, xylylene diisocyanate, vinyl polysiloxane, 2-hydroxypropionic acid and graphene oxide into the obtained mixture, and oscillating and dispersing for 3h under the ultrasonic wave with the power of 500W to form a blend;
step two, adding the blend into a stirrer, adjusting the pH value to 7.8 under the condition that the stirring speed is 120r/min, then heating to 210 ℃ at the heating rate of 4 ℃/min, adding the ethylene-vinyl acetate copolymer and coniferyl alcohol, and keeping the temperature for 50 min;
step three, adding other residual raw material components into the product obtained in the step two, adjusting the pH value to 5.5 under the condition that the stirring speed is 150r/min, then cooling to 145 ℃ at the cooling speed of 1 ℃/min, and then preserving heat for 30 min;
and step four, foaming the product obtained in the step three in a foaming furnace with the frequency of 2200MHz and the power of 5kW for 12min, and then drying in an oven for 5h to obtain the heat-conducting connecting foam.
Example 6
The embodiment provides a heat conduction connection foam, and the raw material composition includes by weight: 9 parts of polycarbonate diol, 13 parts of xylylene diisocyanate, 6 parts of vinyl polysiloxane, 3 parts of 2-hydroxypropionic acid, 0.8 part of graphene oxide, 25 parts of pentaerythritol, 17 parts of polyethyleneimine, 0.8 part of sodium dodecyl sulfate, 2 parts of N-phenyl-2-naphthylamine, 0.3 part of guar hydroxypropyl trimethyl ammonium chloride, 5 parts of foaming agent dichloromethane, 2.5 parts of curing agent acetic acid, 1.2 parts of flame retardant zinc borate, 14 parts of ethylene-vinyl acetate copolymer, 13 parts of modified carbon fiber, 1.6 parts of coniferyl alcohol, 1.3 parts of cashew nut oil and 6 parts of phenolic resin.
According to the raw materials, the preparation method provided by the invention is adopted to prepare the heat-conducting connecting foam:
the method comprises the following steps: uniformly mixing modified carbon fibers, cashew nut oil and phenolic resin, adjusting the pH value to 8.2, heating at 170 ℃ for 45min, adding polycarbonate diol, xylylene diisocyanate, vinyl polysiloxane, 2-hydroxypropionic acid and graphene oxide into the obtained mixture, and oscillating and dispersing for 2.5h under ultrasonic waves with the power of 450W to form a blend;
step two, adding the blend into a stirrer, adjusting the pH value to 7.6 under the condition that the stirring speed is 110r/min, then heating to 210 ℃ at the heating rate of 3 ℃/min, adding the ethylene-vinyl acetate copolymer and coniferyl alcohol, and keeping the temperature for 45 min;
step three, adding other residual raw material components into the product obtained in the step two, adjusting the pH value to 5.0 under the condition that the stirring speed is 140r/min, then cooling to 142 ℃ at the cooling speed of 0.8 ℃/min, and then preserving heat for 25 min;
and step four, foaming the product obtained in the step three in a foaming furnace with the frequency of 2100MHz and the power of 4.5kW for 11min, and then drying in an oven for 4.5h to obtain the heat-conducting connecting foam.
Comparative example 1
This comparative example provides a heat conduction connection bubble is cotton, and the raw materials component includes by weight: 9 parts of polycarbonate diol, 13 parts of xylylene diisocyanate, 6 parts of vinyl polysiloxane, 3 parts of 2-hydroxypropionic acid, 0.8 part of graphene oxide, 25 parts of pentaerythritol, 17 parts of polyethyleneimine, 0.8 part of sodium dodecyl sulfate, 2 parts of N-phenyl-2-naphthylamine, 0.3 part of guar gum hydroxypropyl trimethyl ammonium chloride, 5 parts of foaming agent dichloromethane, 2.5 parts of curing agent acetic acid and 1.2 parts of flame retardant zinc borate.
Preparing heat-conducting connecting foam according to the raw materials:
oscillating and dispersing polycarbonate diol, xylylene diisocyanate, vinyl polysiloxane, 2-hydroxypropionic acid and graphene oxide for 2.5 hours under ultrasonic waves with power of 450W to form a blend; adding the blend into a stirrer, adjusting the pH value to 7.6 under the condition that the stirring speed is 110r/min, then heating to 210 ℃ at the heating rate of 3 ℃/min, and preserving the heat for 45 min; and then adding other residual raw material components, cooling to 142 ℃ at a cooling rate of 0.8 ℃/min under the condition of a stirring rate of 140r/min, preserving the temperature for 25min, foaming for 11min in a foaming furnace with a frequency of 2100MHz and a power of 4.5kW, and drying for 4.5h in an oven to obtain the heat-conducting connecting foam.
Comparative example 2
This comparative example provides a heat conduction connection bubble is cotton, and the raw materials component includes by weight: 9 parts of polycarbonate diol, 13 parts of xylylene diisocyanate, 6 parts of vinyl polysiloxane, 3 parts of 2-hydroxypropionic acid, 0.8 part of graphene oxide, 25 parts of pentaerythritol, 17 parts of polyethyleneimine, 0.8 part of sodium dodecyl sulfate, 2 parts of N-phenyl-2-naphthylamine, 0.3 part of guar hydroxypropyl trimethyl ammonium chloride, 5 parts of foaming agent dichloromethane, 2.5 parts of curing agent acetic acid, 1.2 parts of flame retardant zinc borate, 14 parts of ethylene-vinyl acetate copolymer, 13 parts of modified carbon fiber, 1.6 parts of coniferyl alcohol and 6 parts of phenolic resin.
Preparing heat-conducting connecting foam according to the raw materials:
the method comprises the following steps: uniformly mixing modified carbon fibers, cashew nut oil and phenolic resin, adjusting the pH value to 8.2, heating at 170 ℃ for 45min, adding polycarbonate diol, xylylene diisocyanate, vinyl polysiloxane, 2-hydroxypropionic acid and graphene oxide into the obtained mixture, and oscillating and dispersing for 2.5h under ultrasonic waves with the power of 450W to form a blend;
step two, adding the blend into a stirrer, adjusting the pH value to 7.6 under the condition that the stirring speed is 110r/min, then heating to 210 ℃ at the heating rate of 3 ℃/min, adding the ethylene-vinyl acetate copolymer and coniferyl alcohol, and keeping the temperature for 45 min;
step three, adding other residual raw material components into the product obtained in the step two, adjusting the pH value to 5.0 under the condition that the stirring speed is 140r/min, then cooling to 142 ℃ at the cooling speed of 0.8 ℃/min, and then preserving heat for 25 min;
and step four, foaming the product obtained in the step three in a foaming furnace with the frequency of 2100MHz and the power of 4.5kW for 11min, and then drying in an oven for 4.5h to obtain the heat-conducting connecting foam.
Comparative example 3
This comparative example provides a heat conduction connection bubble is cotton, and the raw materials component includes by weight: 9 parts of polycarbonate diol, 13 parts of xylylene diisocyanate, 6 parts of vinyl polysiloxane, 3 parts of 2-hydroxypropionic acid, 0.8 part of graphene oxide, 25 parts of pentaerythritol, 17 parts of polyethyleneimine, 0.8 part of sodium dodecyl sulfate, 2 parts of N-phenyl-2-naphthylamine, 0.3 part of guar hydroxypropyl trimethyl ammonium chloride, 5 parts of foaming agent dichloromethane, 2.5 parts of curing agent acetic acid, 1.2 parts of flame retardant zinc borate, 14 parts of ethylene-vinyl acetate copolymer, 13 parts of modified carbon fiber, 1.6 parts of coniferyl alcohol, 1.3 parts of cashew nut oil and 6 parts of phenolic resin.
Preparing heat-conducting connecting foam according to the raw materials:
the method comprises the following steps: mixing modified carbon fibers, cashew nut oil, phenolic resin, polycarbonate diol, xylylene diisocyanate, vinyl polysiloxane, 2-hydroxypropionic acid and graphene oxide, and then oscillating and dispersing for 2.5 hours under ultrasonic waves with the power of 450W to form a blend;
step two, adding the blend into a stirrer, adjusting the pH value to 7.6 under the condition that the stirring speed is 110r/min, then heating to 210 ℃ at the heating rate of 3 ℃/min, adding the ethylene-vinyl acetate copolymer and coniferyl alcohol, and keeping the temperature for 45 min;
step three, adding other residual raw material components into the product obtained in the step two, adjusting the pH value to 5.0 under the condition that the stirring speed is 140r/min, then cooling to 142 ℃ at the cooling speed of 0.8 ℃/min, and then preserving heat for 25 min;
and step four, foaming the product obtained in the step three in a foaming furnace with the frequency of 2100MHz and the power of 4.5kW for 11min, and then drying in an oven for 4.5h to obtain the heat-conducting connecting foam.
Comparative example 4
This comparative example provides a heat conduction connection bubble is cotton, and the raw materials component includes by weight: 9 parts of polycarbonate diol, 13 parts of xylylene diisocyanate, 6 parts of vinyl polysiloxane, 3 parts of 2-hydroxypropionic acid, 0.8 part of graphene oxide, 25 parts of pentaerythritol, 17 parts of polyethyleneimine, 0.8 part of sodium dodecyl sulfate, 2 parts of N-phenyl-2-naphthylamine, 0.3 part of guar hydroxypropyl trimethyl ammonium chloride, 5 parts of foaming agent dichloromethane, 2.5 parts of curing agent acetic acid, 1.2 parts of flame retardant zinc borate, 14 parts of ethylene-vinyl acetate copolymer, 13 parts of modified carbon fiber, 1.6 parts of coniferyl alcohol, 1.3 parts of cashew nut oil and 6 parts of phenolic resin.
Preparing heat-conducting connecting foam according to the raw materials:
the method comprises the following steps: uniformly mixing modified carbon fibers, cashew nut oil and phenolic resin, heating at 170 ℃ for 45min, adding polycarbonate diol, xylylene diisocyanate, vinyl polysiloxane, 2-hydroxypropionic acid and graphene oxide into the obtained mixture, and oscillating and dispersing for 2.5h under ultrasonic waves with the power of 450W to form a blend;
step two, adding the blend into a stirrer, heating to 210 ℃ at a heating rate of 3 ℃/min under the condition that the stirring speed is 110r/min, adding the ethylene-vinyl acetate copolymer and coniferyl alcohol, and keeping the temperature for 45 min;
step three, adding other residual raw material components into the product obtained in the step two, cooling to 142 ℃ at a cooling rate of 0.8 ℃/min under the condition that the stirring rate is 140r/min, and then preserving heat for 25 min;
and step four, foaming the product obtained in the step three in a foaming furnace with the frequency of 2100MHz and the power of 4.5kW for 11min, and then drying in an oven for 4.5h to obtain the heat-conducting connecting foam.
The heat-conducting connecting foam prepared in the embodiments 1 to 6 of the present invention was systematically evaluated for its effect through tests, and the heat-conducting connecting foam prepared in the comparative examples 1 to 4 and two commercially available types of heat-conducting foam were used as controls.
1. Determination of thermal conductivity
The heat conductivity coefficient of the heat-conducting connecting foam prepared in the embodiments 1 to 6 and the comparative examples 1 to 4 of the present invention was measured, the reference groups were commercially available heat-conducting foam a and heat-conducting foam B, the measurement method adopted was a method commonly used in the industry, the heat conductivity coefficient in the test results was 100% of the result of the embodiment 1, the results of the other groups were calculated ratios with respect to the result of the embodiment 1, and the test results are shown in the following table 1.
TABLE 1 measurement results of thermal conductivity
| Group of | Example 1 | Example 2 | Example 3 |
| Coefficient of thermal conductivity | 100.00% | 98.53% | 102.57% |
| Group of | Example 4 | Example 5 | Example 6 |
| Coefficient of thermal conductivity | 144.85% | 142.28% | 145.59% |
| Group of | Comparative example 1 | Comparative example 2 | Comparative example 3 |
| Coefficient of thermal conductivity | 78.68% | 81.25% | 87.43% |
| Group of | Comparison ofExample 4 | Commercially available heat-conducting foam A | Commercial heat-conducting foam B |
| Coefficient of thermal conductivity | 68.75% | 74.63% | 55.15% |
2. Compression resilience performance, waterproof performance, flame retardant performance and temperature equalization performance
The heat-conducting connecting foam prepared in the embodiments 1 to 6 and the comparative examples 1 to 4 of the invention is subjected to measurement of compression resilience, waterproof performance, flame retardant performance and temperature uniformity, and the comparison groups are commercially available heat-conducting foam A and heat-conducting foam B. The waterproof performance test is a standard test strictly according to IEC 60529 edition2.1:2001-02IPX2 by using a rain test box, and the measurement method adopted by other performances is a method commonly used in the industry, wherein the compression resilience refers to the elastic recovery condition after compressing heat-conducting connecting foam by 50%, then releasing the pressure for 2min and repeating for 100 times (100% means that the elasticity is recovered to the first compression), the flame retardant performance in the test results is 100% of the result of the example 1, and the results of other groups are calculated ratios relative to the result of the example 1, and the specific results are shown in the following table 2.
TABLE 2 measurement results of thermal conductivity compression resilience, water resistance, flame retardancy, and temperature uniformity
| Group of | Example 1 | Example 2 | Example 3 |
| Compression resilience performance | 88.5% | 88.4% | 88.9% |
| Water resistance | No water infiltration | No water infiltration | No water infiltration |
| Flame retardant properties | 100% | 99.9% | 100.2% |
| Temperature equalizing performance | Good taste | Good taste | Good taste |
| Group of | Example 4 | Example 5 | Example 6 |
| Compression resilience performance | 100% | 100% | 100% |
| Water resistance | No water infiltration | No water infiltration | No water infiltration |
| Flame retardant properties | 100.1% | 100.2% | 100.2% |
| Temperature equalizing performance | Good effect | Good effect | Good effect |
| Group of | Comparative example 1 | Comparative example 2 | Comparative example 3 |
| Compression resilience performance | 78.5% | 74.7% | 78.2% |
| Water resistance | No water infiltration | No water infiltration | Penetration of trace amounts of water |
| Flame retardant properties | 100.1% | 98.9% | 92.7% |
| Temperature equalizing performance | Good effect | In | Is poor |
| Group of | Comparative example 4 | Commercially available heat-conducting foam A | Commercial heat-conducting foam B |
| Compression resilience performance | 53.2% | 71.7% | 46.4% |
| Water resistance | Penetration of trace amounts of water | Small amount of water infiltration | Small amount of water infiltration |
| Flame retardant properties | 88.4% | 100% | 100% |
| Temperature equalizing performance | Is poor | Difference (D) | Is poor |
From the results, the heat-conducting connecting foam provided by the invention has the advantages that under the synergistic effect of the components, through a specific preparation process, including specific temperature rise programs, pH values, temperature reduction programs, charging sequences and the like of all steps, the prepared heat-conducting connecting foam has high heat conductivity coefficient, good temperature uniformity, high internal foaming rate of the foam, uniform and fine foam holes, stable performance in all aspects, excellent compression resilience, flame retardance, waterproofness and structural stability, and the comprehensive effect is far better than that of the foam provided in a comparative example and two types of commercially available heat-conducting foam, so that the heat-conducting connecting foam has a good application prospect.
It should be noted that the polycarbonate diol used in the examples and comparative examples of the present invention was PCD L-1000, the vinyl polysiloxane was vinyl terminated polydimethylsiloxane having a vinyl content of 0.3%, CAS number of 2-hydroxypropionic acid was 50-21-5, CAS number of pentaerythritol was 115-77-5, CAS number of polyethyleneimine was 9002-98-6, CAS number of sodium dodecyl sulfate was 151-21-3, molecular weight of N-phenyl-2-naphthylamine was 177.2429, melting point was 108 ℃, EINECS number of guar hydroxypropyltrimonium chloride was 232-536-8, foaming agent was dichloromethane, curing agent was acetic acid, flame retardant was zinc borate, mass content of vinyl acetate in ethylene-vinyl acetate copolymer (EVA) was 33%, melt index at 190 ℃ was 43g/10min, CAS number of coniferyl alcohol was 458-35-5, and CAS number of phenolic resin was 9003-35-4.
It is to be noted that, unless otherwise specified, technical or scientific terms used herein shall have the ordinary meaning as understood by those skilled in the art to which the invention pertains. Unless specifically stated otherwise, the relative steps, numerical expressions, and values of the components and steps set forth in these embodiments do not limit the scope of the present invention. In all examples shown and described herein, unless otherwise specified, any particular value should be construed as merely illustrative, and not restrictive, and thus other examples of example embodiments may have different values.
In the description of the present invention, it is to be understood that the terms "first", "second" and the like are used for descriptive purposes only and are not to be construed as indicating or implying relative importance or implying any number of technical features indicated. Thus, a feature defined as "first" or "second" may explicitly or implicitly include one or more of that feature. In the description of the present invention, "a plurality" means two or more unless specifically defined otherwise.
Finally, it should be noted that: the above embodiments are only used to illustrate the technical solution of the present invention, and not to limit the same; while the invention has been described in detail and with reference to the foregoing embodiments, it will be understood by those skilled in the art that: the technical solutions described in the foregoing embodiments may still be modified, or some or all of the technical features may be equivalently replaced; the modifications or the substitutions do not make the essence of the corresponding technical solutions depart from the scope of the technical solutions of the embodiments of the present invention, and all of the technical solutions are covered in the protective scope of the present invention.
Claims (10)
1. The heat-conducting connecting foam is characterized by comprising the following raw material components in parts by weight:
8-10 parts of polycarbonate diol, 12-15 parts of xylylene diisocyanate, 4-9 parts of vinyl polysiloxane, 2-4 parts of 2-hydroxypropionic acid, 0.6-1.0 part of graphene oxide, 20-30 parts of pentaerythritol, 15-20 parts of polyethyleneimine, 0.5-1 part of sodium dodecyl sulfate, 1-3 parts of N-phenyl-2-naphthylamine, 0.1-0.4 part of guar gum hydroxypropyl trimethyl ammonium chloride, 3-8 parts of a foaming agent, 2-3 parts of a curing agent and 1-1.5 parts of a flame retardant.
2. The thermally conductive connecting foam of claim 1, wherein the raw material components further comprise:
12-15 parts of ethylene-vinyl acetate copolymer, 10-16 parts of modified carbon fiber, 1-2 parts of coniferyl alcohol, 1-1.5 parts of cashew nut oil and 5-7 parts of phenolic resin.
3. The heat-conducting connecting foam cotton is characterized by comprising the following raw material components in parts by weight:
9 parts of polycarbonate diol, 13 parts of xylylene diisocyanate, 6 parts of vinyl polysiloxane, 3 parts of 2-hydroxypropionic acid, 0.8 part of graphene oxide, 25 parts of pentaerythritol, 17 parts of polyethyleneimine, 0.8 part of sodium dodecyl sulfate, 2 parts of N-phenyl-2-naphthylamine, 0.3 part of guar gum hydroxypropyl trimethyl ammonium chloride, 5 parts of a foaming agent, 2.5 parts of a curing agent, 1.2 parts of a flame retardant, 14 parts of an ethylene-vinyl acetate copolymer, 13 parts of modified carbon fibers, 1.6 parts of coniferyl alcohol, 1.3 parts of cashew nut oil and 6 parts of phenolic resin.
4. The thermally conductive connecting foam of claim 2, wherein:
the preparation method of the modified carbon fiber comprises the following steps: mixing carbon fiber and p-aminobenzoic acid in a ratio of 1: (40-50), adding a sodium hydroxide solution at the temperature of 190-210 ℃ for reaction for 45-60h, adding acetic acid to adjust the pH value to 4-4.5, standing for 80-100h, and drying to obtain the modified carbon fiber.
5. The thermally conductive connecting foam of claim 2, wherein:
the preparation method of the cashew nut oil comprises the following steps: mixing cashew nut kernels and an ethanol water solution in a proportion of 100: (40-50), and heating at 80-95 ℃ for 60-70min to obtain a cashew nut mixture; crushing cashew shell to a particle size of less than 0.2mm, and then drying until the water content is not higher than 3% to obtain cashew shell powder; and uniformly mixing the cashew nut mixture and the cashew nut shell powder, then squeezing at the temperature of 45-50 ℃ by adopting a double-screw oil press, filtering the obtained crude oil, and collecting filtrate to obtain the cashew nut oil.
6. The thermally conductive connecting foam of claim 5, wherein:
the volume fraction of ethanol in the ethanol aqueous solution is 65-75%; the mass ratio of the cashew nut mixture to the cashew nut shell powder is 1: (2-3).
7. The preparation method of the heat-conducting connecting foam cotton as claimed in claim 1, characterized by comprising the following steps:
carrying out oscillation dispersion on polycarbonate diol, xylylene diisocyanate, vinyl polysiloxane, 2-hydroxy propionic acid and graphene oxide for 2-3h under the ultrasonic wave with the power of 400-500W to form a blend; adding the blend into a stirrer, adjusting the pH value to 7.5-7.8 under the condition that the stirring speed is 100-120r/min, then heating to 210 ℃ at the heating rate of 2-4 ℃/min, and preserving the heat for 40-50 min; then adding other residual raw material components, adjusting the pH value to 4.5-5.5 under the condition that the stirring speed is 130-plus-150 r/min, cooling to 140-plus-145 ℃ at the cooling speed of 0.5-1 ℃/min, then preserving the temperature for 20-30min, then foaming for 10-12min in a foaming furnace with the frequency of 2000-plus-2200 MHz and the power of 4-5kW, and then drying for 4-5h in an oven to obtain the heat-conducting connecting foam.
8. The preparation method of the heat-conducting connecting foam cotton as claimed in any one of claims 2 to 6, characterized by comprising the following steps:
the method comprises the following steps: uniformly mixing modified carbon fiber, cashew nut oil and phenolic resin, adjusting the pH value to 8.0-8.4, then heating at 180 ℃ for 40-50min, adding polycarbonate diol, xylylene diisocyanate, vinyl polysiloxane, 2-hydroxypropionic acid and graphene oxide into the obtained mixture, and oscillating and dispersing for 2-3h under the ultrasonic wave with the power of 400 DEG and 500W to form a blend;
step two, adding the blend into a stirrer, adjusting the pH value to 7.5-7.8, then heating to 210 ℃, adding ethylene-vinyl acetate copolymer and coniferyl alcohol, and keeping the temperature for 40-50 min;
step three, adding other residual raw material components into the product obtained in the step two, adjusting the pH value to 4.5-5.5, then cooling to 140-145 ℃, and then preserving heat for 20-30 min;
and step four, foaming the product obtained in the step three in a foaming furnace with the frequency of 2000-2200MHz and the power of 4-5kW for 10-12min, and then drying in an oven for 4-5h to obtain the heat-conducting connecting foam.
9. The method for preparing the heat-conducting connecting foam cotton according to claim 8, characterized in that:
in the second step, the stirring speed is 100-120r/min, and the heating rate of the temperature rise is 2-4 ℃/min.
10. The method for preparing the heat-conducting connecting foam cotton according to claim 8, characterized in that:
in the third step, the stirring speed is 130-150r/min, and the cooling speed of cooling is 0.5-1 ℃/min.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202010386345.0A CN111500048A (en) | 2020-05-09 | 2020-05-09 | Heat-conducting connecting foam and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202010386345.0A CN111500048A (en) | 2020-05-09 | 2020-05-09 | Heat-conducting connecting foam and preparation method thereof |
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Cited By (1)
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| CN113307937A (en) * | 2021-05-26 | 2021-08-27 | 湖北祥源新材科技股份有限公司 | In-situ flame-retardant reinforced polyurethane foam and preparation method thereof |
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