CN115785886A - High-elongation bi-component polyurethane structural adhesive suitable for bonding power batteries and preparation method thereof - Google Patents
High-elongation bi-component polyurethane structural adhesive suitable for bonding power batteries and preparation method thereof Download PDFInfo
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- CN115785886A CN115785886A CN202211484259.9A CN202211484259A CN115785886A CN 115785886 A CN115785886 A CN 115785886A CN 202211484259 A CN202211484259 A CN 202211484259A CN 115785886 A CN115785886 A CN 115785886A
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Images
Classifications
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
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- Adhesives Or Adhesive Processes (AREA)
Abstract
The invention provides a high-elongation bi-component polyurethane structural adhesive suitable for bonding a power battery, which comprises the following components in percentage by volume (0.8-1.2): 1, a component A and a component B; the component A comprises: 20-40 parts of modified castor oil; 1-10 parts of micromolecular glycol chain extender; 1-10 parts of rotaxane structure; 40-80 parts of organic nitrogen-phosphorus high-molecular flame-retardant filler; 0.5-5 parts of white carbon black thixotropic agent; 0.3 to 3 weight portions of silane coupling agent; 0.01 to 1 part by weight of a metal catalyst; 0.1 to 2 weight portions of blue color paste; the component B comprises: 20-40 parts by weight of polymer polyisocyanate; 5-20 parts of polyether glycol; 40-80 parts by weight of organic nitrogen-phosphorus high-molecular flame-retardant filler; 0.5-3 parts of 4A molecular sieve water absorbent; 0.5-5 parts of white carbon black thixotropic agent; 0.1 to 2 portions of yellow color paste. The unique rotaxane structure is introduced into the double-component polyurethane structural adhesive, so that the double-component polyurethane structural adhesive provides higher elongation at break on the basis of meeting the requirements of structural adhesion and body strength, and is particularly suitable for structural adhesion in power batteries.
Description
Technical Field
The invention relates to the technical field of adhesives, in particular to a high-elongation bi-component polyurethane structural adhesive suitable for bonding power batteries and a preparation method thereof.
Background
In the field of power batteries, customers have increasingly strict requirements on double-component polyurethane structural adhesive; the adhesive is required to have high body strength and strong base material bonding force, and simultaneously, the cured adhesive has good tensile property and high elongation at break.
At present, in the field of bi-component polyurethane adhesives, three methods are mainly used for improving the elongation at break, namely, a plasticizer is added; secondly, the crosslinking density of the resin is reduced, namely more difunctional polyol is adopted to replace polyfunctional polyol resin; thirdly, the molecular weight of the polyol is improved, and the proportion of soft segments in the system is increased. However, all three methods soften the cured glue, sacrificing bulk strength and reducing the ability to bond to the substrate to some extent. Specifically, the plasticizer is added to destroy hydrogen bonds between molecular chains, and simultaneously has a certain disentanglement effect on a high molecular chain, so that the strength of the adhesive is greatly reduced; reducing the functionality of the polyol can reduce the crosslinking density of the whole three-dimensional network structure, so that the adhesive is softened, and the glass transition temperature of the product is reduced, so that the high-temperature resistance of the product is weakened; although the increase of the molecular weight of the polyol can ensure the bulk strength and simultaneously improve the elongation at break, the increase of the molecular weight can cause the rapid increase of the viscosity of a system and seriously affect the workability of the product.
Disclosure of Invention
In view of the above, the present invention provides a high-elongation two-component polyurethane structural adhesive for bonding a power battery and a preparation method thereof, and the high-elongation two-component polyurethane structural adhesive for bonding a power battery provided by the present invention can improve the elongation at break of an adhesive without sacrificing the body strength and the bonding strength.
The invention provides a high-elongation bi-component polyurethane structural adhesive suitable for bonding a power battery, which comprises the following components in percentage by volume (0.8-1.2): 1, a component A and a component B;
the component A comprises:
20-40 parts of modified castor oil;
1-10 parts of micromolecular glycol chain extender;
1-10 parts of rotaxane structure;
40-80 parts by weight of organic nitrogen-phosphorus high-molecular flame-retardant filler;
0.5-5 parts of white carbon black thixotropic agent;
0.3 to 3 weight portions of silane coupling agent;
0.01 to 1 part by weight of a metal catalyst;
0.1-2 parts of blue color paste;
the component B comprises:
20-40 parts of polymer polyisocyanate;
5-20 parts of polyether glycol;
40-80 parts by weight of organic nitrogen-phosphorus high-molecular flame-retardant filler;
0.5-3 parts of 4A molecular sieve water absorbent;
0.5-5 parts of white carbon black thixotropic agent;
0.1 to 2 portions of yellow color paste.
Preferably, the A component consists of the following components:
29-33 parts of modified castor oil;
5-7 parts of micromolecular glycol chain extender;
2-6 parts of rotaxane structure;
50-60 parts by weight of organic nitrogen-phosphorus high-molecular flame-retardant filler;
1-3 parts of white carbon black thixotropic agent;
0.5 to 1.5 weight portions of silane coupling agent;
0.05 to 0.15 weight portion of metal catalyst;
0.5 to 1.5 portions of blue color paste.
Preferably, the component B consists of the following components:
25-35 parts by weight of polymer polyisocyanate;
8-12 parts of polyether glycol;
50-60 parts of organic nitrogen-phosphorus high-molecular flame-retardant filler;
1.5-2.5 parts by weight of 4A molecular sieve water absorbent;
1-3 parts of white carbon black thixotropic agent;
0.5 to 1.5 portions of yellow color paste.
Preferably, the preparation method of the rotaxane structure specifically comprises the following steps:
the cyclodextrin and the polyether glycol are mixed according to the material quantity equivalent (1-10): 1 in water, then removing the water and finally drying to obtain the rotaxane structure.
Preferably, the cyclodextrin is selected from one or more of alpha-cyclodextrin, beta-cyclodextrin and gamma-cyclodextrin;
the average molecular weight of the polyether diol is 400-12000.
Preferably, the reaction temperature is 20-30 ℃, the stirring speed is 100-300 rpm, and the time is 1-4 h.
Preferably, the water is removed by rotary evaporation; the vacuum degree of the rotary evaporation is less than or equal to-0.09 MPa, the temperature is 50-70 ℃, and the rotating speed is 30-50 rpm.
Preferably, the drying mode is vacuum drying; the temperature of the vacuum drying is 70-90 ℃, the vacuum degree is less than or equal to-0.09 MPa, and the time is 10-15 h.
The invention also provides a preparation method of the high-elongation double-component polyurethane structural adhesive for bonding the power battery, which comprises the following steps:
a) Heating modified castor oil, a small molecular glycol chain extender, a rotaxane structure, an organic nitrogen-phosphorus high-molecular flame-retardant filler, a white carbon black thixotropic agent and a silane coupling agent to 110-130 ℃ under stirring, dehydrating for 1.5-2.5 h under the vacuum condition of less than or equal to-0.09 MPa, then cooling to less than or equal to 50 ℃, adding a metal catalyst and blue color paste, and continuously stirring for 0.5-1 h under the vacuum condition of less than or equal to-0.09 MPa to obtain a component A;
b) Stirring polymer polyisocyanate and polyether glycol at 20-30 ℃, vacuumizing to be less than or equal to-0.09 MPa, reacting for 1-3 h, then adding organic nitrogen phosphorus high-molecular flame-retardant filler, 4A molecular sieve water removal agent and white carbon black thixotropic agent, adding yellow color paste, stirring at 20-30 ℃, vacuumizing to be less than or equal to-0.09 MPa, reacting for 0.5-1.5 h, and obtaining a component B;
c) The component A and the component B are mixed according to the volume ratio (0.8-1.2): 1, uniformly mixing to obtain the high-elongation bi-component polyurethane structural adhesive suitable for bonding power batteries;
the step a) and the step b) are not limited in order.
Preferably, before the organic nitrogen and phosphorus high-molecular flame-retardant filler, the 4A molecular sieve water removing agent and the white carbon black thixotropic agent are added in the step b), the method further comprises the following steps:
drying and dehydrating the organic nitrogen-phosphorus high-molecular flame-retardant filler, the 4A molecular sieve water absorbent and the white carbon black thixotropic agent in a drying room at the temperature of between 90 and 110 ℃ for 20 to 30 hours.
The invention provides a high-elongation bi-component polyurethane structural adhesive suitable for bonding a power battery, which comprises the following components in percentage by volume (0.8-1.2): 1, a component A and a component B; the component A comprises: 20-40 parts of modified castor oil; 1-10 parts of micromolecular diol chain extender; 1-10 parts of rotaxane structure; 40-80 parts by weight of organic nitrogen-phosphorus high-molecular flame-retardant filler; 0.5-5 parts of white carbon black thixotropic agent; 0.3 to 3 weight portions of silane coupling agent; 0.01 to 1 part by weight of a metal catalyst; 0.1-2 parts of blue color paste; the component B comprises: 20-40 parts by weight of polymer polyisocyanate; 5-20 parts of polyether glycol; 40-80 parts by weight of organic nitrogen-phosphorus high-molecular flame-retardant filler; 0.5-3 parts of 4A molecular sieve water absorbent; 0.5-5 parts of white carbon black thixotropic agent; 0.1 to 2 portions of yellow color paste. Compared with the prior art, the unique rotaxane structure is introduced into the double-component polyurethane structural adhesive, the adoption of a traditional plasticizer or the reduction of the crosslinking density is avoided, the whole interaction is realized by matching with other specific components with specific contents, the product provides higher elongation at break on the basis of meeting the requirements of structural bonding and body strength, and the double-component polyurethane structural adhesive is particularly suitable for structural bonding in a power battery. Experimental results show that the tensile shear strength of the two-component polyurethane structural adhesive provided by the invention is 10.7-10.9 MPa (25 ℃,7 d), the bulk tensile strength is 10.9-11.4 MPa (25 ℃,7 d), the elongation at break is 35-63% (25 ℃,7 d), and the elastic modulus is 670-700 MPa (25 ℃,7 d).
In addition, the preparation method provided by the invention has the advantages of easily available raw materials, simple operation, mild conditions and excellent industrial application prospect.
Drawings
FIG. 1 is a schematic diagram of the "rotaxane" structure for improving elongation at break.
Detailed Description
The technical solutions of the present invention will be described clearly and completely with reference to the following embodiments of the present invention, and it should be understood that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
The invention provides a high-elongation bi-component polyurethane structural adhesive suitable for bonding a power battery, which comprises the following components in percentage by volume (0.8-1.2): 1, a component A and a component B;
the component A comprises:
20-40 parts of modified castor oil;
1-10 parts of micromolecular glycol chain extender;
1-10 parts of rotaxane structure;
40-80 parts by weight of organic nitrogen-phosphorus high-molecular flame-retardant filler;
0.5-5 parts of white carbon black thixotropic agent;
0.3 to 3 weight portions of silane coupling agent;
0.01 to 1 part by weight of a metal catalyst;
0.1-2 parts of blue color paste;
the component B comprises:
20-40 parts by weight of polymer polyisocyanate;
5-20 parts of polyether glycol;
40-80 parts by weight of organic nitrogen-phosphorus high-molecular flame-retardant filler;
0.5-3 parts of 4A molecular sieve water absorbent;
0.5-5 parts of white carbon black thixotropic agent;
0.1 to 2 portions of yellow color paste.
In the invention, the high-elongation double-component polyurethane structural adhesive suitable for bonding the power battery comprises the following components in percentage by volume (0.8-1.2): 1, preferably the component A and the component B are prepared from (0.8-1.2): 1, more preferably a component and a component B, in a volume ratio of 1:1, component A and component B.
In the present invention, the a component includes:
20-40 parts of modified castor oil;
1-10 parts of micromolecular glycol chain extender;
1-10 parts of rotaxane structure;
40-80 parts by weight of organic nitrogen-phosphorus high-molecular flame-retardant filler;
0.5 to 5 portions of white carbon black thixotropic agent;
0.3 to 3 weight portions of silane coupling agent;
0.01 to 1 part by weight of a metal catalyst;
0.1-2 parts of blue color paste;
preferably consisting of:
29-33 parts of modified castor oil;
5-7 parts of micromolecular diol chain extender;
2-6 parts of rotaxane structure;
50-60 parts by weight of organic nitrogen-phosphorus high-molecular flame-retardant filler;
1-3 parts of white carbon black thixotropic agent;
0.5 to 1.5 weight portions of silane coupling agent;
0.05 to 0.15 weight portion of metal catalyst;
0.5 to 1.5 portions of blue color paste.
In the present invention, the B component includes:
20-40 parts by weight of polymer polyisocyanate;
5-20 parts of polyether glycol;
40-80 parts by weight of organic nitrogen-phosphorus high-molecular flame-retardant filler;
0.5-3 parts of 4A molecular sieve water absorbent;
0.5-5 parts of white carbon black thixotropic agent;
0.1 to 2 portions of yellow color paste;
preferably consisting of:
25-35 parts by weight of polymer polyisocyanate;
8-12 parts of polyether glycol;
50-60 parts by weight of organic nitrogen-phosphorus high-molecular flame-retardant filler;
1.5-2.5 parts by weight of 4A molecular sieve water absorbent;
1-3 parts of white carbon black thixotropic agent;
0.5 to 1.5 portions of yellow color paste.
The sources of the modified castor oil, the micromolecular diol chain extender, the organic nitrogen-phosphorus high-molecular flame-retardant filler, the white carbon black thixotropic agent, the silane coupling agent, the metal catalyst, the blue color paste, the polymer polyisocyanate, the polyether glycol, the 4A molecular sieve water absorbent and the yellow color paste are not particularly limited, and the modified castor oil, the micromolecular diol chain extender, the organic nitrogen-phosphorus high-molecular flame-retardant filler, the white carbon black thixotropic agent, the silane coupling agent, the metal catalyst, the blue color paste, the polymer polyisocyanate, the polyether glycol, the 4A molecular sieve water absorbent and the yellow color paste can be obtained by adopting commercial products well known by the technical personnel in the field.
In the present invention, the preparation method of the "rotaxane" structure is preferably specifically:
the cyclodextrin and the polyether glycol are mixed according to the material quantity equivalent (1-10): 1 in water, then removing the water and finally drying to obtain the rotaxane structure.
In the present invention, the cyclodextrin is preferably selected from one or more of α -cyclodextrin, β -cyclodextrin, γ -cyclodextrin, more preferably β -cyclodextrin; the polyether glycol preferably has an average molecular weight of 400 to 12000, more preferably 1000 to 3000. The source of the cyclodextrin and the polyether glycol is not particularly limited in the present invention, and commercially available products well known to those skilled in the art may be used.
In the present invention, the reaction temperature is preferably 20 to 30 ℃, the stirring speed is preferably 100 to 300rpm, more preferably 200rpm, and the time is preferably 1 to 4 hours, more preferably 2 to 3 hours.
In the present invention, the water is preferably removed by rotary evaporation, which is a rotary evaporator well known to those skilled in the art; the vacuum degree of the rotary evaporation is preferably less than or equal to-0.09 MPa, the temperature is preferably 50-70 ℃, more preferably 60 ℃, and the rotating speed is preferably 30-50 rpm, more preferably 40rpm.
In the present invention, the drying mode is preferably vacuum drying, and a vacuum drying oven well known to those skilled in the art can be adopted; the temperature of the vacuum drying is preferably 70-90 ℃, more preferably 80 ℃, the vacuum degree is preferably less than or equal to-0.09 MPa, and the time is preferably 10-15 h, more preferably 12-13 h.
Aiming at the technical problem that the elongation at break of the adhesive is improved while the body strength and the bonding strength are not sacrificed, the invention introduces the rotaxane structure into the formula, develops a method for introducing the mechanical interlocking structure rotaxane into a polyurethane framework, and improves the elongation at break of the cured adhesive while maintaining high body strength; the so-called "rotaxane" structure, that is, a plurality of cyclic structures such as cyclodextrin are introduced into the polyether polyol polymer chain, and these cyclic structures may be further reacted with the isocyanate curing agent component; the advantage of introducing such a structure is that when an external force is applied to the polyurethane skeleton, the rings on the polymer chain can slip, and this process can absorb a large amount of energy and give the polyurethane skeleton sufficient deformation capability, thereby greatly increasing the elongation at break of the product.
In the present invention, a schematic diagram of the "rotaxane" structure for improving the elongation at break is shown in fig. 1.
The invention also provides a preparation method of the high-elongation double-component polyurethane structural adhesive for bonding the power battery, which comprises the following steps:
a) Heating modified castor oil, a small molecular glycol chain extender, a rotaxane structure, an organic nitrogen-phosphorus high-molecular flame-retardant filler, a white carbon black thixotropic agent and a silane coupling agent to 110-130 ℃ under stirring, dehydrating for 1.5-2.5 h under the vacuum condition of less than or equal to-0.09 MPa, then cooling to less than or equal to 50 ℃, adding a metal catalyst and blue color paste, and continuously stirring for 0.5-1 h under the vacuum condition of less than or equal to-0.09 MPa to obtain a component A;
b) Stirring polymer polyisocyanate and polyether glycol at 20-30 ℃, vacuumizing to be less than or equal to-0.09 MPa, reacting for 1-3 h, then adding organic nitrogen phosphorus high-molecular flame-retardant filler, 4A molecular sieve water removal agent and white carbon black thixotropic agent, adding yellow color paste, stirring at 20-30 ℃, vacuumizing to be less than or equal to-0.09 MPa, reacting for 0.5-1.5 h, and obtaining a component B;
c) Mixing the component A and the component B according to the volume ratio (0.8-1.2): 1, uniformly mixing to obtain the high-elongation double-component polyurethane structural adhesive suitable for bonding power batteries;
the step a) and the step b) are not limited in order.
In the invention, before the organic nitrogen phosphorus high molecular flame retardant filler, the 4A molecular sieve water removal agent and the white carbon black thixotropic agent are added, the preferable method further comprises the following steps:
drying and dehydrating the organic nitrogen-phosphorus high-molecular flame-retardant filler, the 4A molecular sieve water absorbent and the white carbon black thixotropic agent in a drying room at the temperature of between 90 and 110 ℃ for 20 to 30 hours;
more preferably:
drying and dehydrating the organic nitrogen-phosphorus high-molecular flame-retardant filler, the 4A molecular sieve water absorbent and the white carbon black thixotropic agent in a drying room at 100 ℃ for 24 hours.
The preparation method provided by the invention has the advantages of easily available raw materials, simple operation, mild conditions and excellent industrial application prospect.
Aiming at the technical problem of how to improve the elongation at break, the traditional thinking can be that the elongation at break can be improved only by softening the rubber, and after all, the toughness and the strength are not compatible with each other for the elastomer; on the basis of the above, people can consider weakening the intermolecular interaction by adding a plasticizer or reducing the crosslinking density so as to soften the glue and realize the toughness of the glue; according to the invention, by adding the movable chain segment, energy can be absorbed through intermolecular slippage under the action of external force, and excellent deformability is provided for the polymer skeleton, so that intramolecular interaction is not required to be destroyed, the deformability of the adhesive is greatly improved, and finally, the elongation at break is improved without sacrificing the strength and hardness of the body. Therefore, the invention realizes the technical effect of improving the elongation at break of the adhesive on the basis of not sacrificing the strength of the body and the bonding strength.
The invention provides a high-elongation bi-component polyurethane structural adhesive suitable for bonding a power battery, which comprises the following components in percentage by volume (0.8-1.2): 1, a component A and a component B; the component A comprises: 20-40 parts of modified castor oil; 1-10 parts of micromolecular glycol chain extender; 1-10 parts of rotaxane structure; 40-80 parts by weight of organic nitrogen-phosphorus high-molecular flame-retardant filler; 0.5-5 parts of white carbon black thixotropic agent; 0.3 to 3 weight portions of silane coupling agent; 0.01 to 1 part by weight of a metal catalyst; 0.1-2 parts of blue color paste; the component B comprises: 20-40 parts of polymer polyisocyanate; 5-20 parts of polyether glycol; 40-80 parts by weight of organic nitrogen-phosphorus high-molecular flame-retardant filler; 0.5-3 parts of 4A molecular sieve water absorbent; 0.5-5 parts of white carbon black thixotropic agent; 0.1 to 2 portions of yellow color paste. Compared with the prior art, the unique rotaxane structure is introduced into the double-component polyurethane structural adhesive, the adoption of a traditional plasticizer or the reduction of the crosslinking density is avoided, the whole interaction is realized by matching with other specific components with specific contents, the product provides higher elongation at break on the basis of meeting the requirements of structural bonding and body strength, and the double-component polyurethane structural adhesive is particularly suitable for structural bonding in a power battery. Experimental results show that the tensile shear strength of the two-component polyurethane structural adhesive provided by the invention is 10.7-10.9 MPa (25 ℃,7 d), the bulk tensile strength is 10.9-11.4 MPa (25 ℃,7 d), the elongation at break is 35-63% (25 ℃,7 d), and the elastic modulus is 670-700 MPa (25 ℃,7 d).
In addition, the preparation method provided by the invention has the advantages of easily available raw materials, simple operation, mild conditions and excellent industrial application prospect.
To further illustrate the present invention, the following examples are provided for illustration. The raw materials used in the following examples of the present invention are all commercially available products; wherein, the rotaxane structure is obtained according to the following preparation method:
dispersing 113g of beta-cyclodextrin in 200mL of water in a 500mL single-neck flask, then adding 200g of polyether glycol (molecular weight is 2000, and trademark is Tantainan C2020), and stirring and reacting at 25 ℃ at the rotating speed of 200rpm for 2h; after the reaction is finished, removing water in the flask by a rotary evaporator, setting the vacuum degree to be less than or equal to-0.09 MPa, the temperature to be 60 ℃ and the rotating speed to be 40rpm; finally, the residual liquid is put into a vacuum drying oven and dried for 12 hours under the conditions of 80 ℃ and the vacuum degree of less than or equal to-0.09 MPa to obtain a white powdery rotaxane structure.
The performance test method adopted by the invention is as follows:
tensile shear strength: the tensile shear strength of the GB/T7124-2008 adhesive is measured (rigid material to rigid material), the test base material is 3003Al, and the bonding thickness is 0.2mm;
tensile strength and elongation at break of the body: GB/T528-2009 vulcanized rubber or thermoplastic rubber tensile stress strain performance determination, wherein the thickness of an I-type sample strip is 2mm, and the tensile speed is 100mm/min;
modulus of elasticity: and testing by adopting a DMA (direct memory access) equipment stretching mode, wherein the thickness of a sample strip is 1mm, the scanning frequency is 1Hz, and the heating rate of a heating mode is 1 ℃/min.
Example 1
And (2) component A: the material comprises, by weight, italian modified castor oil H-368 parts, chain extender EHD 6 parts, rotaxane structure 2 parts, foshan Jin Ge JAZ-004 flame-retardant powder 55 parts, CABOT TS720 white carbon black 2 parts, KH-560 silane coupling agent 1 part, united states Van & ltRussian & gt Coscat-83 catalyst 0.1 part, and Baumeishi blue color paste 1 part;
and B component: 30 parts of cigarette platform Wanhua PM-200 polymer polyisocyanate, 10 parts of cigarette platform Wanhua C2020 polyether glycol, 55 parts of Fushan gold Ge JAZ-004 flame-retardant powder, 2 parts of 4A molecular sieve, 2 parts of CABOT TS720 white carbon black and 1 part of Baumei yellow color paste.
Example 2
The component A comprises: the material comprises, by weight, ivy modified castor oil H-368, chain extender EHD 6, rotaxane structure 4, fushan Jin Ge JAZ-004 flame-retardant powder 55, CABOT TS720 white carbon black 2, KH-560 silane coupling agent 1, united states Vateluos Coscat-83 catalyst 0.1 and Baumeishi blue color paste 1;
and B component: 30 parts of cigarette platform Wanhua PM-200 polymer polyisocyanate, 10 parts of cigarette platform Wanhua C2020 polyether glycol, 55 parts of Fushan gold Ge JAZ-004 flame-retardant powder, 2 parts of 4A molecular sieve, 2 parts of CABOT TS720 white carbon black and 1 part of Baumei yellow color paste.
Example 3
The component A comprises: the material comprises, by weight, ivy modified castor oil H-368 29 parts, a chain extender EHD 6 parts, a rotaxane structure 6 parts, fushan gold Ge JAZ-004 flame-retardant powder 55 parts, CABOT TS720 white carbon black 2 parts, KH-560 silane coupling agent 1 part, american Van Te Lus Coscat-83 catalyst 0.1 part, and Baumei blue color paste 1 part;
and B component: 30 parts of cigarette platform Wanhua PM-200 polymer polyisocyanate, 10 parts of cigarette platform Wanhua C2020 polyether glycol, 55 parts of Fushan gold Ge JAZ-004 flame-retardant powder, 2 parts of 4A molecular sieve, 2 parts of CABOT TS720 white carbon black and 1 part of Baumei yellow color paste.
Comparative example 1
The component A comprises: the material comprises, by weight, 35 parts of ethylene glycol modified castor oil H-368, 6 parts of chain extender EHD, 55 parts of Fushan gold-Ge JAZ-004 flame-retardant powder, 2 parts of CABOT TS720 white carbon black, 1 part of KH-560 silane coupling agent, 0.1 part of American Vatelus Coscat-83 catalyst and 1 part of Baumei blue color paste;
and B component: 30 parts of cigarette platform Wanhua PM-200 polymer polyisocyanate, 10 parts of cigarette platform Wanhua C2020 polyether glycol, 55 parts of Fushan gold Ge JAZ-004 flame-retardant powder, 2 parts of 4A molecular sieve, 2 parts of CABOT TS720 white carbon black and 1 part of Baumei yellow color paste.
Comparative example 2
The component A comprises: the material comprises, by weight, 35 parts of ethylene glycol modified castor oil H-368, 6 parts of chain extender EHD, 55 parts of Fushan gold-Ge JAZ-004 flame-retardant powder, 2 parts of CABOT TS720 white carbon black, 1 part of KH-560 silane coupling agent, 0.1 part of American Vatelus Coscat-83 catalyst and 1 part of Baumei blue color paste;
and the component B comprises: 30 parts of cigarette platform Wanhua PM-200 polymer polyisocyanate, 10 parts of cigarette platform Wanhua C2020 polyether diol, 45 parts of Foshan gold GoJAZ-004 flame-retardant powder, 10 parts of DINP plasticizer, 2 parts of 4A molecular sieve, 2 parts of CABOT TS720 white carbon black and 1 part of Baumei yellow color paste.
Comparative example 3
The component A comprises: 25 parts of ethylene glycol modified castor oil H-368, 10 parts of Vatelus D-290 bifunctional modified castor oil, 6 parts of chain extender EHD, 55 parts of Fushan gold Go JAZ-004 flame-retardant powder, 2 parts of CABOT TS720 white carbon black, 1 part of KH-560 silane coupling agent, 0.1 part of American Vatelus Coscat-83 catalyst and 1 part of Baumei blue paste;
and the component B comprises: 30 parts of cigarette platform Wanhua PM-200 polymer polyisocyanate, 10 parts of cigarette platform Wanhua C2020 polyether glycol, 55 parts of Fushan gold Ge JAZ-004 flame-retardant powder, 2 parts of 4A molecular sieve, 2 parts of CABOT TS720 white carbon black and 1 part of Baumei yellow color paste.
The selection and proportion of the components of examples 1 to 3 and comparative examples 1 to 3 are shown in Table 1.
TABLE 1 ingredient selection and proportioning data Table for examples 1-3 and comparative examples 1-3
The preparation method of the two-component polyurethane structural adhesive related to the test comprises the following steps:
(1) Heating modified castor oil, a micromolecular diol chain extender, a rotaxane structure, an organic nitrogen-phosphorus high-molecular flame-retardant filler, a white carbon black thixotropic agent and a silane coupling agent to 120 ℃ under stirring, vacuumizing to-0.09 MPa, dehydrating for 2 hours, then cooling to below 50 ℃, adding a metal catalyst and blue color paste, vacuumizing to-0.09 MPa, and continuously stirring for 45 minutes to obtain a component A.
(2) Firstly, drying and dehydrating organic nitrogen-phosphorus high-molecular flame-retardant filler, a 4A molecular sieve water absorbent and a white carbon black thixotropic agent in a drying room at 100 ℃ for 24 hours for later use; stirring and vacuumizing polymer polyisocyanate and polyether glycol at normal temperature to-0.09 MPa for reaction for 2 hours, then adding pre-dried nitrogen and phosphorus high-molecular flame-retardant filler, a 4A molecular sieve water removal agent and a white carbon black thixotropic agent, adding yellow color paste, stirring and vacuumizing at normal temperature to-0.09 MPa for reaction for 1 hour, and obtaining a component B.
(3) Mixing the component A and the component B according to the volume ratio of 1:1, uniformly mixing to obtain the double-component polyurethane structural adhesive.
In the above test, different parts by mass of "rotaxane" structures were added in example 1, example 2 and example 3, respectively, in comparative example 1, no "rotaxane" structure was added, in comparative example 2, 10 parts of a plasticizer was additionally added to the B component except for the a component to which the "rotaxane" structure was not added, and in comparative example 3, 10 parts of bifunctional modified castor oil was substituted for the a component except for the a component to which the "rotaxane" structure was not added.
The two-component polyurethane structural adhesives prepared in the above examples 1 to 3 and comparative examples 1 to 3 were subjected to various performance tests, and the results are shown in table 2.
TABLE 2 Performance data of examples 1 to 3 and comparative examples 1 to 3
| Performance index | Example 1 | Example 2 | Example 3 | Comparative example 1 | Comparative example 2 | Comparative example 3 |
| Tensile shear strength (MPa, 25 ℃ C.) | 10.7 | 10.9 | 10.9 | 10.8 | 7.3 | 8.1 |
| Tensile shear strength (MPa, 60 ℃ C.) | 5.9 | 6.5 | 6.4 | 6.3 | 4.1 | 4.8 |
| Bulk tensile Strength (MPa, 25 ℃ C.) | 11.0 | 10.9 | 11.4 | 11.5 | 7.9 | 8.5 |
| Elongation at Break (%, 25 ℃ C.) | 35 | 57 | 63 | 28 | 60 | 52 |
| Bulk tensile Strength (MPa, 60 ℃ C.) | 6.9 | 7.1 | 7.1 | 7.3 | 4.5 | 5.3 |
| Elongation at Break (%, 60 ℃ C.) | 62 | 89 | 99 | 49 | 105 | 97 |
| Modulus of elasticity (MPa, 25 ℃ C.) | 680 | 670 | 700 | 730 | 490 | 530 |
| Modulus of elasticity (MPa, 60 ℃ C.) | 85 | 79 | 87 | 89 | 52 | 61 |
The previous description of the disclosed embodiments is provided to enable any person skilled in the art to make or use the present invention. Various modifications to these embodiments will be readily apparent to those skilled in the art, and the generic principles defined herein may be applied to other embodiments without departing from the spirit or scope of the invention. Thus, the present invention is not intended to be limited to the embodiments shown herein but is to be accorded the widest scope consistent with the principles and novel features disclosed herein.
Claims (10)
1. A high-elongation bi-component polyurethane structural adhesive suitable for bonding power batteries comprises the following components in percentage by volume (0.8-1.2): 1, a component A and a component B;
the component A comprises:
20-40 parts of modified castor oil;
1-10 parts of micromolecular glycol chain extender;
1-10 parts of rotaxane structure;
40-80 parts by weight of organic nitrogen-phosphorus high-molecular flame-retardant filler;
0.5-5 parts of white carbon black thixotropic agent;
0.3 to 3 weight portions of silane coupling agent;
0.01 to 1 part by weight of a metal catalyst;
0.1 to 2 weight portions of blue color paste;
the component B comprises:
20-40 parts by weight of polymer polyisocyanate;
5-20 parts of polyether glycol;
40-80 parts by weight of organic nitrogen-phosphorus high-molecular flame-retardant filler;
0.5-3 parts of 4A molecular sieve water absorbent;
0.5-5 parts of white carbon black thixotropic agent;
0.1 to 2 portions of yellow color paste.
2. The high-elongation two-component polyurethane structural adhesive suitable for bonding power batteries according to claim 1, wherein the component A comprises the following components:
29-33 parts of modified castor oil;
5-7 parts of micromolecular glycol chain extender;
2-6 parts of rotaxane structure;
50-60 parts by weight of organic nitrogen-phosphorus high-molecular flame-retardant filler;
1-3 parts of white carbon black thixotropic agent;
0.5 to 1.5 weight portions of silane coupling agent;
0.05 to 0.15 weight portion of metal catalyst;
0.5 to 1.5 portions of blue color paste.
3. The high-elongation two-component polyurethane structural adhesive suitable for bonding power batteries according to claim 1, wherein the component B consists of the following components:
25-35 parts by weight of polymer polyisocyanate;
8-12 parts of polyether glycol;
50-60 parts by weight of organic nitrogen-phosphorus high-molecular flame-retardant filler;
1.5-2.5 parts by weight of 4A molecular sieve water absorbent;
1-3 parts of white carbon black thixotropic agent;
0.5 to 1.5 portions of yellow color paste.
4. The high-elongation bi-component polyurethane structural adhesive suitable for bonding power batteries according to claim 1, wherein the preparation method of the rotaxane structure comprises the following specific steps:
the cyclodextrin and the polyether glycol are mixed according to the material quantity equivalent (1-10): 1 in water, then removing the water and finally drying to obtain the rotaxane structure.
5. The high-elongation two-component polyurethane structural adhesive suitable for bonding power batteries according to claim 4, wherein the cyclodextrin is selected from one or more of alpha-cyclodextrin, beta-cyclodextrin and gamma-cyclodextrin;
the average molecular weight of the polyether diol is 400-12000.
6. The high-elongation bi-component polyurethane structural adhesive suitable for bonding power batteries according to claim 4, wherein the reaction temperature is 20-30 ℃, the stirring speed is 100-300 rpm, and the reaction time is 1-4 h.
7. The high-elongation two-component polyurethane structural adhesive suitable for bonding power batteries according to claim 4, wherein the water is removed by spin steaming; the vacuum degree of the rotary evaporation is less than or equal to-0.09 MPa, the temperature is 50-70 ℃, and the rotating speed is 30-50 rpm.
8. The high-elongation two-component polyurethane structural adhesive suitable for bonding power batteries according to claim 4, wherein the drying manner is vacuum drying; the temperature of the vacuum drying is 70-90 ℃, the vacuum degree is less than or equal to-0.09 MPa, and the time is 10-15 h.
9. A method for preparing the high-elongation two-component polyurethane structural adhesive suitable for bonding the power battery according to any one of claims 1 to 8, which comprises the following steps:
a) Heating modified castor oil, a small molecular glycol chain extender, a rotaxane structure, an organic nitrogen-phosphorus high-molecular flame-retardant filler, a white carbon black thixotropic agent and a silane coupling agent to 110-130 ℃ under stirring, dehydrating for 1.5-2.5 h under the vacuum condition of less than or equal to-0.09 MPa, then cooling to less than or equal to 50 ℃, adding a metal catalyst and blue color paste, and continuously stirring for 0.5-1 h under the vacuum condition of less than or equal to-0.09 MPa to obtain a component A;
b) Stirring polymer polyisocyanate and polyether glycol at 20-30 ℃, vacuumizing to be less than or equal to-0.09 MPa, reacting for 1-3 h, then adding organic nitrogen phosphorus high-molecular flame-retardant filler, 4A molecular sieve water removal agent and white carbon black thixotropic agent, adding yellow color paste, stirring at 20-30 ℃, vacuumizing to be less than or equal to-0.09 MPa, reacting for 0.5-1.5 h, and obtaining a component B;
c) Mixing the component A and the component B according to the volume ratio (0.8-1.2): 1, uniformly mixing to obtain the high-elongation double-component polyurethane structural adhesive suitable for bonding power batteries;
the step a) and the step b) are not limited in order.
10. The preparation method according to claim 9, wherein before the organic nitrogen phosphorus polymer flame retardant filler, the 4A molecular sieve water removal agent and the white carbon black thixotropic agent are added in the step b), the method further comprises the following steps:
drying and dehydrating the organic nitrogen-phosphorus high-molecular flame-retardant filler, the 4A molecular sieve water absorbent and the white carbon black thixotropic agent in a drying room at the temperature of between 90 and 110 ℃ for 20 to 30 hours.
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| CN103361003A (en) * | 2012-03-28 | 2013-10-23 | 琳得科株式会社 | Adhesive composition, adhesive, and adhesive sheet |
| CN107109051A (en) * | 2015-01-13 | 2017-08-29 | 高级软质材料株式会社 | Thermoplastic elastomer (TPE) composition, thermoplastic elastomer (TPE) and method for producing thermoplastic elastomer |
| CN111909337A (en) * | 2020-08-14 | 2020-11-10 | 广州市白云化工实业有限公司 | Crosslinking agent, polyurethane prepolymer and single-component polyurethane adhesive |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2013061988A1 (en) * | 2011-10-28 | 2013-05-02 | 宇部興産株式会社 | Aqueous polyurethane resin dispersion composition |
| CN103361003A (en) * | 2012-03-28 | 2013-10-23 | 琳得科株式会社 | Adhesive composition, adhesive, and adhesive sheet |
| CN107109051A (en) * | 2015-01-13 | 2017-08-29 | 高级软质材料株式会社 | Thermoplastic elastomer (TPE) composition, thermoplastic elastomer (TPE) and method for producing thermoplastic elastomer |
| CN111909337A (en) * | 2020-08-14 | 2020-11-10 | 广州市白云化工实业有限公司 | Crosslinking agent, polyurethane prepolymer and single-component polyurethane adhesive |
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