CN117777928A - Hot-melt bi-component polyurethane heat-conducting structural adhesive, preparation method thereof and gluing method - Google Patents
Hot-melt bi-component polyurethane heat-conducting structural adhesive, preparation method thereof and gluing method Download PDFInfo
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- CN117777928A CN117777928A CN202311858446.3A CN202311858446A CN117777928A CN 117777928 A CN117777928 A CN 117777928A CN 202311858446 A CN202311858446 A CN 202311858446A CN 117777928 A CN117777928 A CN 117777928A
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- Polyurethanes Or Polyureas (AREA)
- Adhesives Or Adhesive Processes (AREA)
Abstract
The invention relates to the technical field of polyurethane adhesives, in particular to a hot-melt bi-component polyurethane heat-conducting structural adhesive, a preparation method thereof and a sizing method thereof, wherein the heat-conducting structural adhesive comprises an A component and a B component, and the A component comprises the following components in percentage by mass: hydroxyl end-capped polyurethane prepolymer, chain extender, heat conducting powder and auxiliary agent A; the component B comprises the following components in percentage by mass: NCO-terminated polyurethane prepolymer, isocyanate, heat conducting powder and an auxiliary agent B. The bi-component structural adhesive has high viscosity at room temperature, can not be used for sizing, is easy to store, is stable in dispersion, is not easy to settle and heat in a product, has moderate viscosity (5-40 ten thousand cps) after being heated to 40-90 ℃, and can be used for sizing normally. The invention solves the problem of storage stability of the polyurethane heat conduction structure used at normal temperature with conventional low viscosity by improving the colloid formula and increasing the sizing temperature, has outstanding mechanical property and excellent bonding property, has large plastic space, and is more suitable for industrial continuous production.
Description
Technical Field
The invention relates to the technical field of polyurethane adhesives, in particular to a hot-melt bi-component polyurethane heat-conducting structural adhesive, a preparation method thereof and a sizing method thereof.
Background
The existing power battery is generally bonded and sealed by adopting a heat-conducting adhesive, and the double-component polyurethane heat-conducting structural adhesive plays an important role, but also provides higher requirements on the performance of the adhesive, such as high temperature resistance, heat conductivity, environmental protection and safety, storage stability of the adhesive, construction viscosity, operation time, moisture sensitivity, rapid curing, rapid strength establishment and the like.
With the development of mass production technology of power batteries, when the conventional heat-conducting structural adhesive is applied to the production technology of the power batteries, the adhesive needs to be applied within 30 minutes, the shearing strength reaches 0.5Mpa in 1 hour, and the requirements of the next step of working procedures and the improvement of the overall production efficiency can be met, but the conventional heat-conducting structural adhesive generally adopts a room-temperature adhesive mode, the structural adhesive is quite easy to settle and laminate, the upper layer has low viscosity, the lower layer is possibly hardened, the stability of the use of customers is influenced, the influence on the performance is quite large, the storage period is short, the contradiction between the viscosity and the room-temperature storage period cannot be effectively balanced, the production requirements of long operation time and quick positioning cannot be met, the requirement of moisture sensitivity of a component B can be met with high cost, and the room-temperature curing toughness is poor, so the development of the polyurethane heat-conducting structural adhesive suitable for the adhesion of the power batteries is needed,
disclosure of Invention
Aiming at the problems, the invention provides a hot-melt bi-component polyurethane heat-conducting structural adhesive which has excellent mechanical properties and construction manufacturability. The bi-component structural adhesive has high viscosity at room temperature, can not be applied with glue, is easy to store, is stable in dispersion and is not easy to settle in a product, and has moderate viscosity (5-40 ten thousand cps) after being heated to 40-90 ℃ and can be applied with glue normally. The invention solves the problem of storage stability of the polyurethane heat conduction structure used at normal temperature with conventional low viscosity by improving the colloid formula and increasing the sizing temperature, has outstanding mechanical property and excellent bonding property, has large plastic space, and is more suitable for industrial continuous production.
In order to achieve the technical purpose, one scheme of the application is as follows:
the hot-melt bi-component polyurethane heat-conducting structural adhesive comprises an A component and a B component, wherein the A component comprises the following components in percentage by mass: 8-50% of hydroxyl-terminated polyurethane prepolymer, 45-90% of heat conducting powder and 0.2-5% of auxiliary agent A, wherein the auxiliary agent A comprises at least one of dispersing agent, thixotropic agent, plasticizer and catalyst; the component B comprises the following components in percentage by mass: 8-50% of NCO-terminated polyurethane prepolymer, 45-90% of heat conducting powder and 0.2-8% of auxiliary agent B, wherein the auxiliary agent B comprises at least one of a water removing agent, a thixotropic agent and a coupling agent.
From the above description, it can be seen that this formulation has the following advantages:
the hydroxyl-terminated polyurethane prepolymer in the component A is an important component of the component A, which can obtain key mechanical properties, and when the polymer polyol and isocyanate are controllably crosslinked, the main chain of the polyol has strong activity capability, and the viscosity fluctuation along with the change of temperature is large, the adhesive can be smoothly discharged after slightly heating.
The component A and the component B of the hot-melt double-component polyurethane heat-conducting structural adhesive are viscous liquid or waxy solid at room temperature, have no fluidity or slight fluidity, so that the A, B component can be ensured to have enough storage period at room temperature and not to be easily separated out in a layering manner like the common double-component heat-conducting adhesive, and the stability of the colloid quality is affected. The heat conduction structural adhesive has the heat conduction coefficient of more than or equal to 0.8w.mk, the viscosity of the mixed adhesive can reach 50000-400000 cps (at the temperature of 40-90 ℃), more preferably 80000-250000 cps (at the temperature of 40-60 ℃), and the mixing effect is excellent.
Preferably, the mixture ratio of the synthetic raw materials of the hydroxyl-terminated polyurethane prepolymer meets NCO/OH < 0.7, and the hydroxyl value of the prepolymer is 60-1000 mgKOH/g; under the condition of relative excessive polyol, the viscosity and the reactivity of the obtained prepolymer can be reasonably regulated, and the viscosity of the colloid at room temperature and high temperature (40-90 ℃) can be considered after the heat conducting powder is added.
Preferably, the hydroxyl terminated polyurethane prepolymer is prepared by reacting a polyol with isocyanate, wherein the polyol adopts at least one of difunctional or trifunctional polyether polyol with molecular weight of 100-3000, difunctional polyester polyol with molecular weight of 100-4000, PTMEG with molecular weight of 500-4000 and polybutadiene polyol, and the isocyanate adopts at least one of polymerization MDI, MDI, TDI, HMDI, IPDI and HDI trimer; the low Tg liquid polyether or long chain carbon-carbon liquid di-or polyol provides excellent flowability of the system, especially at elevated temperatures.
As an improvement, the hydroxyl-terminated polyurethane prepolymer is further added with tackifying resin or crystalline polyester polyol in the synthesis process, the glass transition temperature of the tackifying resin or crystalline polyester polyol is less than 100 ℃, and the addition amount of the tackifying resin or crystalline polyester polyol accounts for 5-30% of the weight of the hydroxyl-terminated polyurethane prepolymer; the addition of tackifying resins or polyester resins can serve to balance the viscosity of the product, provide pressure sensitive properties, and improve the final bond strength.
Preferably, the chain extender comprises a small molecular chain extender, wherein the small molecular chain extender adopts at least one of butanediol, ethylene glycol, diethylene glycol, triethylene glycol, propylene glycol, dipropylene glycol, glycerol, hexanediol, octanediol and neopentyl glycol, and the addition amount of the small molecular chain extender accounts for 1-15% of the weight of the component A; the reaction speed of A, B components after being mixed is effectively controlled, and the final strength and the toughness of the product can be improved by reasonable collocation.
Preferably, the NCO-terminated polyurethane prepolymer has an NCO content of 3 to 28% and is prepared by reacting a polyol comprising at least one of a difunctional or trifunctional polyether polyol having a molecular weight of 100 to 3000, a difunctional polyester polyol having a molecular weight of 100 to 4000, a PTMEG having a molecular weight of 500 to 4000, and a polybutadiene polyol with an isocyanate comprising at least one of HMDI, MDI, liquefied MDI, MDI-50, a polymeric MDI, HDI, HDI trimer, IPDI, XDI, and NDI.
As an improvement, the isocyanate of the component B adopts at least one of HMDI, MDI, liquefied MDI, MDI-50, polymeric MDI, HDI, HDI trimer, IPDI, XDI and NDI; the addition of isocyanate can adjust the equivalent weight of NCO of the component B to form an accurate ratio when matched with the component A; while his presence allows for adjustment of the reactivity of the A, B components after mixing, the curing time and finally the hardness of the product.
Preferably, the heat conductive powder comprises Al 2 O 3 、Al(OH) 3 、ZnO 2 And BN, at least one of; the specific proportion is determined by the requirements of heat conductivity coefficient, system viscosity and the like.
Based on the hot-melt bi-component polyurethane heat-conducting structural adhesive, the application also provides a preparation method of the hot-melt bi-component polyurethane heat-conducting structural adhesive, which comprises the following steps:
s1, weighing raw materials of all components according to the formula proportion;
s2, preparing a component A, namely adding a hydroxyl-terminated polyurethane prepolymer, a chain extender, an auxiliary agent A and heat conducting powder into a planetary stirring device, heating to 30-100 ℃ to uniformly disperse, discharging at 40-90 ℃, and sealing and preserving to obtain the component A;
s3, preparing a component B, namely adding NCO-terminated polyurethane prepolymer, isocyanate, an auxiliary agent B and heat conducting powder into a planetary stirring device, heating to 30-100 ℃ for uniform dispersion, discharging at 40-90 ℃, and sealing and preserving to obtain the component B.
From the above description, it can be seen that this method has the following advantages:
the preparation method is simple, and the properties such as adhesive force, curing speed and the like can be adjusted by hydroxyl terminated polyurethane prepolymer, NCO-terminated polyurethane prepolymer and other components.
Based on the hot-melt bi-component polyurethane heat conduction structural adhesive, the application also provides a sizing method of the hot-melt bi-component polyurethane heat conduction structural adhesive, which comprises the following steps:
and (3) heating the component A and the component B to 40-90 ℃ respectively, mixing the heated component A and the heated component B according to the volume ratio of 1:1, and then sizing, wherein the pressure-sensitive duration is more than 30min.
From the above description, it can be seen that this method has the following advantages:
when the hot-melt double-component polyurethane heat-conducting structural adhesive is used for sizing, the adhesive can be sized only by heating the component A and the component B at a lower temperature (the heating temperature is less than 90 ℃), the component A and the component B are easy to mix in the sizing process, the mixing effect is good, and a good bonding effect can be achieved. The sizing method can meet the requirements that the sizing is carried out within 30min and the shearing strength at 1h can meet the requirement of more than 0.5Mpa in the existing power battery production process, the performance of the battery cannot be affected by sizing at the temperature, the sizing method has reasonable carrying bonding strength, and the production rate of finished products of the battery can be obviously improved.
Detailed Description
The following describes embodiments of the invention in detail, but does not limit the claims of the invention in any way.
In the invention, the following components are added: the hydroxyl value refers to the milligrams of potassium hydroxide (KOH) equivalent to hydroxyl groups in 1g of a sample, expressed in mgKOH/g, and is obtained by testing through a GB 12008.3-89 polyester polyol hydroxyl value measuring method; the method comprises the steps of carrying out a first treatment on the surface of the Viscosity refers to the resistance of a fluid to flow, as measured by a brookfield viscometer; the NCO/OH ratio refers to the molar ratio of the NCO and OH groups of the reaction starting materials during the prepolymer reaction.
The application provides a hot-melt bi-component polyurethane heat-conducting structural adhesive which has high viscosity at room temperature, can not be applied with glue, is easy to store, has moderate viscosity (5-40 ten thousand cps) after being heated to 40-90 ℃, and can be applied with glue normally. The invention solves the problem of storage stability of the conventional polyurethane heat conduction structure by increasing the sizing temperature, has outstanding mechanical properties, and is more suitable for industrial continuous production.
The specific formula is as follows:
a hot-melt bi-component polyurethane heat-conducting structural adhesive comprises a component A and a component B;
wherein:
the component A comprises the following components in percentage by mass:
8-50% of hydroxyl terminated polyurethane prepolymer and chain extender;
45-90% of heat conducting powder;
0.2 to 5 percent of auxiliary agent A;
the component B comprises the following components in percentage by mass:
8-50% of NCO-terminated polyurethane prepolymer and isocyanate;
45-90% of heat conducting powder;
0.2 to 8 percent of auxiliary agent B.
The formula comprises the following components:
the proportion of the synthetic raw materials of the hydroxyl-terminated polyurethane prepolymer should satisfy NCO/OH < 0.7, preferably NCO/OH < 0.5, and the hydroxyl value of the prepolymer should satisfy 60-1000 mgKOH/g, preferably 100-500 mgKOH/g.
Hydroxyl-terminated polyurethane prepolymers can be prepared by reacting polyols with isocyanates; the polyol can be selected from one or more of difunctional or trifunctional polyether polyol with molecular weight of 100-3000, difunctional polyester polyol with molecular weight of 100-4000, PTMEG with molecular weight of 500-4000 and polybutadiene polyol; the isocyanate can be selected to polymerize one or more of MDI, MDI, TDI, HMDI, IPDI and HDI trimer.
The auxiliary agent A comprises a dispersing agent, a thixotropic agent, a plasticizer, a catalyst and the like, and one or more of the auxiliary agents A and the catalyst can be selected.
The chain extender comprises a small molecular chain extender, wherein the small molecular chain extender can be selected from one or more of butanediol, ethylene glycol, diethylene glycol, triethylene glycol, propylene glycol, dipropylene glycol, glycerol, hexanediol, octanediol and neopentyl glycol, and the addition amount of the small molecular chain extender accounts for 1-15% of the weight of the component A, preferably 2-8% of the weight of the component A;
the NCO-terminated polyurethane prepolymer has an NCO content of 3 to 28%, preferably 6 to 24%, more preferably 10 to 20%; NCO-terminated polyurethane prepolymer is prepared by prepolymerizing polyol and isocyanate, wherein NCO/OH is more than 2, the polyol adopts at least one of difunctional or trifunctional polyether polyol with molecular weight of 100-3000, difunctional polyester polyol with molecular weight of 100-4000, PTMEG with molecular weight of 500-4000 and polybutadiene polyol, and the isocyanate adopts at least one of HMDI, MDI, liquefied MDI, MDI-50, polymerized MDI, HDI, HDI trimer, IPDI, XDI and NDI;
the auxiliary agent B comprises a leveling agent, a water removing agent, a dispersing agent, a thixotropic agent, a plasticizer, a coupling agent and the like, and one or more of the auxiliary agents can be selected.
In order to further balance the pressure sensitivity, viscosity and final strength of the hot-melt two-component polyurethane heat-conducting structural adhesive, a tackifying resin or crystalline polyester polyol may also be added during the synthesis of the hydroxyl-terminated polyurethane prepolymer, the softening point or glass transition temperature of the tackifying resin or crystalline polyester polyol being less than 100 ℃, preferably less than 70 ℃, more preferably less than 55 ℃, the tackifying resin or crystalline polyester polyol being added in an amount of 5 to 30 parts by weight, preferably 8 to 20 parts by weight, of the hydroxyl-terminated polyurethane prepolymer. The tackifying resin can be acrylic resin, EVA resin, rosin resin and the like with different molecular weights. The crystalline polyester polyol may be adipic acid series, polyethylene glycol series, polycaprolactone, etc.
In order to further balance the properties of the hot-melt two-component polyurethane heat-conducting structural adhesive, the isocyanate of the component B can be one or more of HMDI, MDI, liquefied MDI, MDI-50, polymeric MDI, HDI, HDI trimer, IPDI, XDI and NDI.
The specific preparation method of the hot-melt bi-component polyurethane heat-conducting structural adhesive comprises the following steps:
s1, weighing raw materials of all components according to the formula proportion;
s2, preparing a component A, namely adding a hydroxyl terminated polyurethane prepolymer, a small molecular chain extender, an auxiliary agent A and heat conducting powder into a planetary stirring device, heating to 30-100 ℃ to uniformly disperse, discharging at 40-90 ℃, and sealing and preserving to obtain the component A;
s3, preparing a component B, namely adding NCO-terminated polyurethane prepolymer, isocyanate, an auxiliary agent B and heat conducting powder into a planetary stirring device, heating to 30-100 ℃ to uniformly disperse, discharging at 40-90 ℃, and sealing and preserving to obtain the component B.
When in use, the component A and the component B are respectively heated to 40-90 ℃ (preferably 40-60 ℃), the heated component A and the heated component B are mixed according to the volume ratio of 1:1, and then sizing is carried out, wherein the pressure-sensitive sustainable time (or pressing time) is more than 30min.
The following gives a formulation table of 4 specific examples based on the formulation and preparation method of the above-mentioned hot-melt two-component polyurethane heat-conducting structural adhesive. And a formulation table of a comparative example of the existing hot-melt two-component polyurethane heat-conducting structural adhesive is provided.
Among the above formulations, the hydroxyl-terminated polyurethane prepolymer in the A-component and the NCO-terminated polyurethane prepolymer in the B-component were formulated as shown in Table 2:
the specific preparation steps of examples 1-4 and comparative example 1 are given below based on the above formulation table:
example 1
And (3) preparing a component A:
preparation of A-component hydroxyl-terminated polyurethane prepolymer
20 parts of castor oil, 9 parts of PEG-400, 20 parts of XCP-1000N (Asahi Sichuan chemical), 20 parts of PTMEG1000 and 20 parts of MN3050D are uniformly mixed in a reaction bottle, 5 parts of BM751 (Shanghai Boli chemical), the mixture is heated to 110 ℃, vacuumized and dehydrated for 2 hours, cooled to 60 ℃,6 parts of CDMDI-100L (Wanhua) are added, and the mixture is heated to 80 ℃ for 2 hours and then sealed and stored.
The following raw materials were uniformly mixed in parts by mass in a planetary mixer, 11.6 parts of the above hydroxyl-terminated polyurethane prepolymer, 9.4 parts of PTMEG1000 (Sanchi Japan), 3.5 parts of MN307 (Lanxingdong), 2 parts of DPG (dipropylene glycol, commercially available), 2 parts of 3A molecular sieve (Shanghai Jiujikui molecular sieve Co., ltd.), 3 parts of submicron Al 2 O 3 18.6 parts of heat conducting powder5 micron Al 2 O 3 63 parts of heat conducting powder, 0.4 part of B11/70 dispersing aid (Kelaien chemical (China) Co., ltd.) and 0.1 part of 8% T-12 (castor oil dilution).
And (2) preparing a component B:
preparation of NCO-terminated polyurethane prepolymers of the B component
10 parts of castor oil, 2 parts of MN3050D (large blue star), 10 parts of PCL210N (large Japanese xylonite) are uniformly mixed in a reaction bottle, heated to 110 ℃, vacuumized and dehydrated for 2 hours, cooled to 60 ℃, 31 parts of PM200 (Wanhua) are added, 47 parts of CDMDI-100L (Wanhua) are added, and the mixture is heated to 80 ℃ to react for 2 hours and then sealed and stored.
14 parts of the NCO-terminated polyurethane prepolymer described above, 2 parts of PM200,2.8 parts of submicron Al 2 O 3 16.7 parts of 5 micrometer Al 2 O 3 The heat conducting powder, 64 parts of heat conducting compound powder and 0.5 part of PTSI water scavenger are added into a planetary mixer for uniform mixing.
A, B components are respectively filled into 1:1 rubber tubes, and are sized after being heated to 40-60 ℃ by a hot melt adhesive gun, and related performance parameters are shown in table 1.
Example 2
And (3) preparing a component A:
preparation of A-component hydroxyl-terminated polyurethane prepolymer
24 parts of castor oil, 15 parts of MN700 (large blue star), 45 parts of PEG400 and 6 parts of XCP-1000N (Xuchuan chemical) are uniformly mixed in a reaction bottle, heated to 110 ℃, vacuumized and dehydrated for 2 hours, cooled to 60 ℃, added with 10 parts of CDMDI-100L (Wanhua), heated to 80 ℃ and reacted for 2 hours, and then sealed and stored.
The following raw materials, by mass, were uniformly mixed in a planetary mixer, 13 parts of the above hydroxyl-terminated polyurethane prepolymer, 3.1 parts of DPG (dipropylene glycol, commercially available), 3.6 parts of 3A molecular sieve (Shanghai Seismic molecular sieve Co., ltd.), 11 parts of 5 μm Al 2 O 3 68 parts of heat conducting powder, 1 part of flame retardant plasticizer IPPP50,0.2 part of fumed silica H20 (Wake chemical) and 0.1 part of 8% T-12 (castor oil dilution).
And (2) preparing a component B:
preparation of NCO-terminated polyurethane prepolymers of the B component
10 parts of MN3050D (Lanxingdong), 15 parts of PTMEG1000 are uniformly mixed in a reaction bottle, heated to 110 ℃, vacuumized and dehydrated for 2 hours, cooled to 60 ℃, 50 parts of PM200 (Wanhua) are added, 25 parts of MDI-50 are heated to 80 ℃ for reaction for 2 hours, and then sealed and stored.
16 parts of the NCO-terminated polyurethane prepolymer, 6 parts of HT-100 (Wanhua), 11 parts of 5-micrometer Al2O3 heat conducting powder, 66.1 parts of heat conducting compound powder, 0.5 part of PTSI water scavenger and 0.4 part of fumed silica H20 are added into a planetary mixer at one time and mixed uniformly.
A, B components are respectively filled into 1:1 rubber hoses, and are sized after being heated to 40-60 ℃ by a hot melt adhesive gun, and relevant performance parameters are shown in table 1.
Example 3
And (3) preparing a component A:
preparation of A-component hydroxyl-terminated polyurethane prepolymer
60 parts of castor oil, 15 parts of MN700 (Lanxingdong), 10 parts of PTMEG1000 and 6 parts of DV-125 (Lanxingdong) are uniformly mixed in a reaction bottle, heated to 110 ℃, vacuumized and dehydrated for 2 hours, cooled to 60 ℃, added with 9 parts of CDMDI-100L (Wanhua), heated to 80 ℃ and reacted for 2 hours, and then sealed and stored.
The following raw materials were uniformly mixed in parts by mass in a planetary mixer, 16.2 parts of the above hydroxyl-terminated polyurethane prepolymer, 2.5 parts of DPG (dipropylene glycol, commercially available), 2 parts of Unilink4200 (Wanhua), 4 parts of 3A molecular sieve (Shanghai Seama molecular sieve Co., ltd.), 74 parts of heat-conducting compound powder, 1 part of plasticizer DUP di-n-undecyl phthalate, 0.2 part of fumed silica H20 (Walch chemical), 0.1 part of 8% T-12 (castor oil dilution).
And (2) preparing a component B:
preparation of NCO-terminated polyurethane prepolymers of the B component
20 parts of PPG1000, 10 parts of BM755 (Shanghai Boril chemical industry), 15 parts of XCP-1000N are uniformly mixed in a reaction bottle, heated to 110 ℃, vacuumized and dehydrated for 2 hours, cooled to 60 ℃, added with 55 parts of MDI-50, heated to 80 ℃ and reacted for 2 hours, and then sealed and stored.
20.5 parts of the NCO-terminated polyurethane prepolymer, 5 parts of PM200, 73 parts of heat-conducting compound powder, 1 part of silane coupling agent KH560 and 0.5 part of PTSI water scavenger are added into a planetary mixer for uniform mixing.
A, B components are respectively filled into 1:1 rubber hoses, and are sized after being heated to 40-60 ℃ by a hot melt adhesive gun, and relevant performance parameters are shown in table 1.
Example 4
And (3) preparing a component A:
preparation of A-component hydroxyl-terminated polyurethane prepolymer
45 parts of castor oil, 16 parts of DL-400 (Lanxingdong), 7 parts of MN3050D and 25 parts of BM751 (Shanghai Boli chemical industry) are uniformly mixed in a reaction bottle, the mixture is heated to 130 ℃, vacuumized and dehydrated for 2 hours, cooled to 60 ℃,7 parts of CDMDI-100L (Wanhua) are added, and the mixture is heated to 80 ℃ for 2 hours and then sealed and stored.
The following raw materials were uniformly mixed in parts by mass in a planetary mixer, 17.2 parts of the above hydroxyl-terminated polyurethane prepolymer, 5 parts of bisphenol a modified polyol DIO235 (shanghai tyl de chemical), 5 parts of triethylene glycol TEG,4 parts of 3A molecular sieve (shanghai long-life molecular sieve limited), 68 parts of heat-conducting compounding powder, 1 part of plasticizer DUP di-n-undecyl phthalate, 0.5 part of fumed silica H20 (wack chemical), 0.3 part of 30% DY-5508 (castor oil dilution, shanghai de sound chemical).
And (2) preparing a component B:
preparation of NCO-terminated polyurethane prepolymers of the B component
Mixing 15 parts of PTMEG1000 and 10 parts of XCP-1000H uniformly in a reaction bottle, heating to 110 ℃, vacuumizing to remove water for 2 hours, cooling to 60 ℃, adding 55 parts of HT-100 and 20 parts of HMDI, heating to 90 ℃, reacting for 2 hours, and sealing for storage.
12 parts of the NCO-terminated polyurethane prepolymer, 19.2 parts of PM200, 67.3 parts of heat-conducting compound powder, 0.5 part of fumed silica H20 and 1.0 part of PTSI water scavenger are added into a planetary mixer at one time and mixed uniformly.
A, B components are respectively filled into 1:1 rubber hoses, and are sized after being heated to 40-60 ℃ by a hot melt adhesive gun, and relevant performance parameters are shown in table 1.
Comparative example 1
And (3) preparing a component A:
preparation of A-component hydroxyl-terminated polyurethane prepolymer
Mixing 25 parts of castor oil, 46 parts of DL-400 (blue star Dong Da), 20 parts of MN700 in a reaction bottle uniformly, heating to 110 ℃, vacuumizing to remove water for 2 hours, cooling to 60 ℃, adding 9 parts of CDMDI-100L (Wanhua), heating to 80 ℃, reacting for 2 hours, and sealing for storage.
The following raw materials, by mass, were uniformly mixed in a planetary mixer, 9.1 parts of the above hydroxyl-terminated polyurethane prepolymer, 1.8 parts of DV-125,2 parts of dipropylene glycol DPG,2 parts of a 3A molecular sieve (Shanghai Jiujiu molecular sieve Co., ltd.), 3 parts of submicron Al2O3 heat conductive powder, 18.6 parts of 5 micron Al2O3 heat conductive powder, 63 parts of heat conductive compound powder, 0.4 part of B11/70 dispersing aid (Clay chemical Co., ltd.), and 0.1 part of 8% T-12 (castor oil dilution).
And (2) preparing a component B:
preparation of NCO-terminated polyurethane prepolymers of the B component
10 parts of castor oil, 2 parts of MN3050D (large blue star) are uniformly mixed in a reaction bottle, heated to 110 ℃, vacuumized and dehydrated for 2 hours, cooled to 60 ℃, 41 parts of PM200 (Wanhua) and 47 parts of CDMDI-100L (Wanhua) are added, heated to 80 ℃ and reacted for 2 hours, and then sealed and stored.
13 parts of the NCO-terminated polyurethane prepolymer, 3 parts of PM200,2.8 parts of submicron Al2O3 heat conducting powder, 16.7 parts of 5 micron Al2O3 heat conducting powder, 64 parts of heat conducting compound powder and 0.5 part of PTSI water scavenger are added into a planetary mixer at one time and uniformly mixed.
A, B components are respectively filled into 1:1 rubber hoses, and are sized after being heated to 40-60 ℃ by a hot melt adhesive gun, and relevant performance parameters are shown in table 1.
Table 1 results of performance testing of various embodiments
Remarks: initial strength refers to the adhesive strength after 10 minutes after application of the glue, the comparative example viscosity test is 25℃at room temperature, and the example is 50 ℃.
From table 1, it can be seen that 4 examples have significant advantages in terms of strength and elongation, and that examples can achieve no precipitation for 6 months, slight precipitation for 1 month of comparative example, and significant precipitation for 3 months, affecting the adhesive performance stability.
In summary, the invention has the following advantages:
1. the double-component heat-conducting structural adhesive is sized by using a heating process, so that the viscosity adjustment range of A, B components is greatly widened, and more adjustable space is increased for improving the performance;
2. a, B can be waxy solid or paste without hands at room temperature, has more excellent long-term storage stability without precipitation, and can reach shelf life of more than 1 year;
3. the B component may have a lower NCO content, more excellent moisture sensitivity, and may use aromatic isocyanates to achieve skin formation times of 16 hours or more;
4. the hot-melt bi-component polyurethane is used for selecting polyurethane raw materials, so that the selection of powder raw materials is wider, and the cost of the raw materials is easier to control;
5. solves the problem that some easily crystallized raw materials can not be used, and enriches the selectivity of the raw materials;
6. the heating sizing process is also suitable for the construction of adhesive systems such as acrylic acid, epoxy, organosilicon and the like;
7. the heating construction process widens the application range of the double-component polyurethane, can make more adjustment on the molecular structure, can realize the application of the heat-conducting polyurethane pressure-sensitive adhesive, can dismantle the heat-conducting structural adhesive, and has high strength and high elongation.
It is to be understood that the foregoing detailed description of the invention is merely illustrative of the invention and is not limited to the embodiments of the invention. It will be understood by those of ordinary skill in the art that the present invention may be modified or substituted for elements thereof to achieve the same technical effects; as long as the use requirement is met, the invention is within the protection scope of the invention.
Claims (10)
1. The hot-melt double-component polyurethane heat-conducting structural adhesive comprises a component A and a component B, and is characterized in that,
the component A comprises the following components in percentage by mass: 8-50% of hydroxyl-terminated polyurethane prepolymer, 45-90% of heat conducting powder and 0.2-5% of auxiliary agent A, wherein the auxiliary agent A comprises at least one of dispersing agent, thixotropic agent, plasticizer and catalyst;
the component B comprises the following components in percentage by mass: 8-50% of NCO-terminated polyurethane prepolymer, 45-90% of heat conducting powder and 0.2-8% of auxiliary agent B, wherein the auxiliary agent B comprises at least one of a water removing agent, a thixotropic agent and a coupling agent.
2. The hot-melt two-component polyurethane heat-conducting structural adhesive according to claim 1, wherein the hydroxyl-terminated polyurethane prepolymer has a synthetic raw material ratio satisfying NCO/OH < 0.7 and a prepolymer hydroxyl value of 60-1000 mgKOH/g.
3. The hot melt two-component polyurethane heat transfer structural adhesive of claim 1, wherein the hydroxyl terminated polyurethane prepolymer is prepared by reacting a polyol with an isocyanate, the polyol is at least one of a difunctional or trifunctional polyether polyol having a molecular weight of 100-3000, a difunctional polyester polyol having a molecular weight of 100-4000, a PTMEG having a molecular weight of 500-4000 and a polybutadiene polyol, and the isocyanate is at least one of a polymer MDI, MDI, TDI, HMDI, IPDI and an HDI trimer.
4. A hot melt two-component polyurethane heat transfer structural adhesive according to claim 3, wherein the hydroxyl terminated polyurethane prepolymer is further added during the synthesis with a tackifying resin or crystalline polyester polyol having a glass transition temperature of less than 100 ℃, the tackifying resin or crystalline polyester polyol being added in an amount of 5-30% by weight of the hydroxyl terminated polyurethane prepolymer.
5. The hot-melt two-component polyurethane heat-conducting structural adhesive according to claim 1, wherein the chain extender comprises a small-molecule chain extender, and the small-molecule chain extender adopts at least one of butanediol, ethylene glycol, diethylene glycol, triethylene glycol, propylene glycol, dipropylene glycol, glycerol, hexanediol, octanediol and neopentyl glycol, and the addition amount of the small-molecule chain extender is 1-15% by weight of the component A.
6. The hot melt two-component polyurethane heat transfer structural adhesive of claim 1, wherein the NCO-terminated polyurethane prepolymer has an NCO content of 3 to 28%;
the NCO-terminated polyurethane prepolymer is prepared by reacting a polyol with isocyanate, wherein the NCO/OH is more than 2, the polyol adopts at least one of difunctional or trifunctional polyether polyol with molecular weight of 100-3000, difunctional polyester polyol with molecular weight of 100-4000, PTMEG with molecular weight of 500-4000 and polybutadiene polyol, and the isocyanate adopts at least one of HMDI, MDI, liquefied MDI, MDI-50, polymerized MDI, HDI, HDI trimer, IPDI, XDI and NDI.
7. The two-component polyurethane heat transfer structural adhesive of claim 6, wherein the isocyanate in the B component is at least one of HMDI, MDI, liquefied MDI, MDI-50, polymeric MDI, HDI, HDI trimer, IPDI, XDI, and NDI.
8. The hot-melt two-component polyurethane heat-conducting structural adhesive according to claim 1, wherein the heat-conducting powder comprises Al 2 O 3 、Al(OH) 3 、ZnO 2 And BN.
9. A method of preparing the hot melt two-component polyurethane heat conductive structural adhesive of any one of claims 1 to 8, comprising the steps of:
s1, weighing raw materials of all components according to the formula proportion;
s2, preparing a component A, namely adding a hydroxyl-terminated polyurethane prepolymer, a chain extender, an auxiliary agent A and heat conducting powder into a planetary stirring device, heating to 30-100 ℃ to uniformly disperse, discharging at 40-90 ℃, and sealing and preserving to obtain the component A;
s3, preparing a component B, namely adding NCO-terminated polyurethane prepolymer, isocyanate, an auxiliary agent B and heat conducting powder into a planetary stirring device, heating to 30-100 ℃ to uniformly disperse, discharging at 40-90 ℃, and sealing and preserving to obtain the component B.
10. A method of sizing a hot melt two-component polyurethane heat transfer structural adhesive as claimed in any one of claims 1 to 8, comprising the steps of:
and (3) heating the component A and the component B to 40-90 ℃ respectively, mixing the heated component A and the heated component B according to the volume ratio of 1:1, and then sizing, wherein the pressure-sensitive duration is more than 30min.
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