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CN107033789B - Insulation protection glue and preparation method and application thereof - Google Patents

Insulation protection glue and preparation method and application thereof Download PDF

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Publication number
CN107033789B
CN107033789B CN201710249281.8A CN201710249281A CN107033789B CN 107033789 B CN107033789 B CN 107033789B CN 201710249281 A CN201710249281 A CN 201710249281A CN 107033789 B CN107033789 B CN 107033789B
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insulation
oligomer
parts
protective adhesive
preheating
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CN107033789A (en
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于爱霞
李利华
郑长利
黄仁杰
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Guangzhou Huili Electronic Material Co ltd
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Guangzhou Huili Electronic Material Co ltd
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    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J4/00—Adhesives based on organic non-macromolecular compounds having at least one polymerisable carbon-to-carbon unsaturated bond ; adhesives, based on monomers of macromolecular compounds of groups C09J183/00 - C09J183/16
    • C09J4/06—Organic non-macromolecular compounds having at least one polymerisable carbon-to-carbon unsaturated bond in combination with a macromolecular compound other than an unsaturated polymer of groups C09J159/00 - C09J187/00
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
    • C09J11/02—Non-macromolecular additives
    • C09J11/06—Non-macromolecular additives organic
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M50/00—Constructional details or processes of manufacture of the non-active parts of electrochemical cells other than fuel cells, e.g. hybrid cells
    • H01M50/10—Primary casings; Jackets or wrappings
    • H01M50/183—Sealing members
    • 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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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Electrochemistry (AREA)
  • General Chemical & Material Sciences (AREA)
  • Adhesives Or Adhesive Processes (AREA)
  • Addition Polymer Or Copolymer, Post-Treatments, Or Chemical Modifications (AREA)

Abstract

The invention relates to an insulation protective adhesive and a preparation method and application thereof, belonging to the technical field of chemical materials. The insulation protection glue is mainly prepared from the following raw materials in parts by weight: 40-55 parts of oligomer, 45-60 parts of active monomer, 3-8 parts of photoinitiator and 0-10 parts of auxiliary agent, wherein the oligomer is polybutadiene acrylate; the active monomer is at least one of monofunctional acrylate and difunctional acrylate. The insulating protective adhesive can be applied by screen printing or spraying and the like, is rapidly cured by UV light, does not need to be attached, and is not limited by shape and size; electrolyte and various acids and alkalis can be endured for a long time, and leakage is prevented; the insulation property is good, the voltage of more than 1000V can be endured, and the electric leakage is prevented; the adhesive force and the wear resistance are good, and the colloid can not fall off or be seriously worn after long-time use. The method can be used for insulation and isolation protection of the surface of the aluminum shell of the power battery, can also be used in other similar applications, and has the advantage of wide application range.

Description

Insulation protection glue and preparation method and application thereof
Technical Field
The invention relates to the technical field of chemical materials, in particular to an insulation protective adhesive and a preparation method and application thereof.
Background
With the increasing energy crisis and environmental pollution, the development of clean pure electric vehicles with high efficiency, energy conservation and zero emission has become a necessary trend for the development of the domestic and foreign automobile industry. In recent years, with the development demand of technology and the strong promotion of system, China has become the highest point of development of electric vehicles all over the world. In 2016, the total sales of Chinese public buses (excluding tourism buses) is about 10 thousands of buses, wherein about 7 thousands of pure electric buses and 1.7 thousands of plug-in hybrid buses account for 87% of the total sales. Meanwhile, the development of the hot tide is also met abroad, the sale of fuel vehicles is basically stopped in 2030 in Norway and the Netherlands, Japan shows that the popularity of the new generation can reach 50% in 2030, and Germany proposes that the investment on the fuel vehicles is not made in 2025.
Therefore, the electric automobile needs a large amount of power batteries, and the market is considerable. The conventional power battery shell is mostly an aluminum shell, and if the battery leaks in the use process, electrolyte, various acids and alkalis and the like can corrode the shell and further corrode other devices; if the outer layer of the aluminum shell has poor insulativity, the aluminum shell is easy to be punctured, and electric leakage is caused. In order to prevent electric leakage and liquid leakage, the surface of the aluminum shell of the battery is required to be insulated or isolated, and the insulation paper is commonly used in the market to achieve the effect. However, the insulating paper is difficult to be attached without gaps and limited by size and model, and with the rapid development of electric automobiles, the defects need to be solved urgently.
Disclosure of Invention
In view of the above, there is a need to provide an insulating protective adhesive, which can be used for insulating and isolating the surface of the aluminum casing of the power battery, and plays a role in insulation and protection.
An insulation protection adhesive is mainly prepared from the following raw materials in parts by weight:
Figure BDA0001271544400000011
Figure BDA0001271544400000021
the oligomer is in polybutadiene acrylate;
the active monomer is at least one of monofunctional acrylate and difunctional acrylate.
The insulating protective adhesive has excellent tolerance to ions, solvents and the like through crosslinking of weak polar macromolecules and the cyclic diluent monomers, and can meet the insulating protection application on the surface of the aluminum shell of the power battery due to excellent insulating property of the material, and can also be used in other similar applications requiring insulation and/or ion or solvent resistance.
In one embodiment, the insulation protection adhesive is mainly prepared from the following raw materials in parts by weight:
Figure BDA0001271544400000022
the insulating protective adhesive prepared according to the formula proportion has better various properties.
In one embodiment, the monofunctional acrylate is selected from: isobornyl methacrylate and/or isobornyl acrylate;
the difunctional acrylate is selected from the group consisting of: tricyclodecane dimethanol diacrylate and/or dioxanone hexadiol diacrylate.
The active monomer has a cyclic structure and good compatibility with the oligomer, and can form an ideal three-dimensional structure by crosslinking with the oligomer after being initiated by the photoinitiator, so that the attack of ions or solvents is blocked, and the active monomer has good tolerance to the oligomer.
In one embodiment, the photoinitiator is at least one of a free radical photoinitiator;
the auxiliary agent is at least one of an adhesion promoter, a defoaming agent and a flatting agent.
The auxiliary agent can be added according to actual production requirements, and the performance of the insulation protective adhesive is improved.
In one embodiment, the free radical photoinitiator is selected from: at least one of alpha-hydroxyketone derivatives, benzoyl formate, acylphosphine oxides, benzophenones and derivatives thereof
In one embodiment, the adhesion promoter is selected from: at least one of gamma-glycidoxypropyltrimethoxysilane, gamma-methacryloxypropyltrimethoxysilane, gamma-methacryloxypropyltriethoxysilane, and a polyfunctional thiol compound;
the defoaming agent is a silicone defoaming agent;
the leveling agent is an organic silicon leveling agent.
The invention also discloses a preparation method of the insulation protection adhesive, which comprises the following steps:
preheating: preheating the oligomer;
and (3) hot mixing: keeping the preheating temperature, adding the active monomer, and completely dissolving the oligomer in the active monomer to obtain a mixed glue solution;
mixing: stopping heating, adding the photoinitiator and the auxiliary agent, and stirring uniformly under the condition of residual heat to obtain the high-performance ultraviolet curing coating.
The preparation method of the insulation protection adhesive has the characteristics of simple process and high reliability, and can be conveniently applied to industrial production.
In one embodiment, the preheating step, wherein the oligomer is heated to 50-70 ℃ for preheating. Preferably 55-65 ℃. The insulating protective adhesive is prepared within the temperature range, so that excellent performance of the insulating protective adhesive can be ensured.
The invention also discloses application of the insulation protection adhesive on the surface of the aluminum shell of the power battery.
The insulation protection glue can replace insulation paper, is applied to power battery aluminum shell insulation or isolation protection, is applied by means of screen printing or spraying and the like, is rapidly cured by UV light, has excellent insulation property due to glue, has excellent tolerance to electrolyte and acid-base, and can prevent leakage of batteries.
Compared with the prior art, the invention has the following beneficial effects:
the insulation protection glue can replace insulation paper, is applied to power battery aluminum shell insulation or isolation protection, is applied by means of screen printing or spraying and the like, is rapidly cured by UV light, and can prevent battery leakage and leakage due to the fact that the glue has excellent insulation property and excellent tolerance to electrolyte and acid and alkali.
The preparation method of the insulation protection adhesive has the characteristics of simple process and high reliability, and can be conveniently applied to industrial production.
The insulating protective adhesive can be applied by screen printing or spraying and the like, is rapidly cured by UV light, does not need to be attached, and is not limited by shape and size; electrolyte and various acids and alkalis can be endured for a long time, and leakage is prevented; the insulation property is good, the voltage of more than 1000V can be endured, and the electric leakage is prevented; the adhesive force and the wear resistance are good, and the colloid can not fall off or be seriously worn after long-time use.
The insulating protective adhesive can be used for insulating and isolating the surface of the aluminum shell of the power battery, can also be used in other similar applications, and has the advantage of wide application range.
Detailed Description
In order that the invention may be more fully understood, reference will now be made to the following description. This invention may, however, be embodied in many different forms and should not be construed as limited to the embodiments set forth herein. Rather, these embodiments are provided so that this disclosure will be thorough and complete.
Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. The terminology used in the description of the invention herein is for the purpose of describing particular embodiments only and is not intended to be limiting of the invention. As used herein, the term "and/or" includes any and all combinations of one or more of the associated listed items.
The color of the insulating protective adhesive described in the following embodiments is colorless and transparent, the coating method of the insulating protective adhesive is screen printing or spraying, or special equipment and process can be adopted, and the curing method of the insulating protective adhesive is UV light curing.
The starting materials used in the following examples are all commercially available.
Example 1
An insulation protective adhesive is a colorless and transparent UV photocuring product and is prepared from the following raw materials:
oligomer: 45.80g in total.
45.80g of polybutadiene acrylate.
Reactive monomer: 45.80g in total.
Monofunctional acrylate, isobornyl acrylate (IBOA)45.80 g.
Photoinitiator (2): 3.59g in total.
13.59g of 2-hydroxy-2-methyl-phenyl-propanone.
Auxiliary agent: total 4.81 g.
Adhesion promoter (gamma-methacryloxypropyltriethoxysilane) 0.72g,
(polyfunctional thiol compound, type PE-1)3.59g,
0.3g of defoaming agent (silicone defoaming agent, model number BYK066N),
0.2g of leveling agent (organic silicon leveling agent, model number SIVEL 5525).
The insulating protective adhesive of the embodiment is prepared by the following method:
firstly, preheating.
Preheating the oligomer.
The method comprises the following specific steps:
45.80g of oligomeric polybutadiene acrylate were placed in a feed vessel and heated to 60 ℃.
Secondly, thermal mixing.
The temperature was maintained at 60 ℃ and the active monomer was added with stirring to dissolve the oligomer completely in the active monomer (active monomer isobornyl acrylate (IBOA)45.80g of monofunctional acrylate) to obtain a mixed gum solution.
And thirdly, mixing.
Stopping heating, adding a photoinitiator and an auxiliary agent (the photoinitiator is 2-hydroxy-2-methyl-phenyl acetone-13.59 g, the adhesion promoter is 0.72g of gamma-methacryloxypropyl triethoxysilane, the polyfunctional group mercaptan compound is 3.59g, the defoaming agent is 0.3g of BYK066N, and the leveling agent is 0.2g of SIVEL 5525), and stirring at a high speed until the mixture is uniform in the residual heat of the previous step; vacuumizing and subpackaging to obtain the colorless and transparent insulating protective adhesive.
The performance test of the insulating protective adhesive has the following results:
the viscosity of the insulating protective adhesive is about 1500cps, and the density is 0.93g/cm3(ii) a The curing energy was 2500mj/cm2The hardness after curing is about 42D; go through baige OK, wear resistant OK; the adhesive layer can resist electrolyte (60 ℃) for more than 10 days when the thickness of the adhesive layer is 100-200 mu m, can resist voltage of more than 1000V, can resist certain acid such as HF, oxalic acid, sulfuric acid and nitric acid, and can resist certain alkali such as sodium hydroxide, potassium hydroxide, TMAH and the like, and the specific details are shown in the following table 1.
Example 2
An insulation protective adhesive is a colorless and transparent UV photocuring product and is prepared from the following raw materials:
oligomer: 45.80g in total.
45.80g of polybutadiene acrylate.
Reactive monomer: 45.80g in total.
Monofunctional acrylate, isobornyl methacrylate (IBOMA)27.48g,
bifunctional acrylate: dicidol diacrylate (18.32 g).
Photoinitiator (2): 3.59g in total.
12.79 g of 2-hydroxy-2-methyl-phenyl acetone,
0.80g of 2,4, 6-trimethylbenzoyl-diphenylphosphine oxide.
Auxiliary agent: total 4.81 g.
0.95g of adhesion promoter (gamma-glycidoxypropyltrimethoxysilane),
(polyfunctional thiol compound, type PE-LED)3.36g,
0.3g of defoaming agent (silicone defoaming agent, model number BYK066N),
0.2g of leveling agent (organic silicon leveling agent, model number SIVEL 5525).
The insulating protective adhesive of the embodiment is prepared by the following method:
firstly, preheating.
Preheating the oligomer.
The method comprises the following specific steps:
45.80g of oligomeric polybutadiene acrylate were placed in a feed vessel and heated to 60 ℃.
Secondly, thermal mixing.
The temperature was maintained at 60 ℃ and the active monomer was added with stirring to dissolve the oligomer completely in the active monomer (isobornyl methacrylate, an active monomer of monofunctional acrylate, 27.48g, tricyclodecane dimethanol diacrylate, an active monomer of difunctional acrylate, 18.32g) to obtain a mixed gum solution.
And thirdly, mixing.
Stopping heating, adding a photoinitiator and an auxiliary agent (the photoinitiator is 2-hydroxy-2-methyl-phenyl acetone-12.79 g, 2,4, 6-trimethylbenzoyl-diphenyl phosphine oxide is 0.80g, the adhesion promoter is gamma-glycidyl ether oxypropyl trimethoxy silane is 0.95g, the polyfunctional group mercaptan compound is 3.36g, the defoaming agent is 0.3g of BYK066N, and the flatting agent is 0.2g of SIVEL 5525), and stirring at a high speed to be uniform in the residual heat of the previous step; vacuumizing and subpackaging to obtain the colorless and transparent insulating protective adhesive.
The performance test of the insulating protective adhesive has the following results:
the viscosity of the insulating protective adhesive is about 2970cps, and the density is 0.93g/cm3(ii) a The curing energy was 2500mj/cm2A hardness of about 64D after curing; go through baige OK, wear resistant OK; the adhesive layer can resist electrolyte (60 ℃) for more than 10 days when the thickness of the adhesive layer is 100-200 mu m, can resist voltage of more than 1000V, can resist certain acid such as HF, oxalic acid, sulfuric acid and nitric acid, and can resist certain alkali such as sodium hydroxide, potassium hydroxide, TMAH and the like, and the specific details are shown in the following table 1.
Comparative example 1
An insulating protective adhesive, which is substantially the same as the insulating protective adhesive of example 1 and is prepared by the preparation method of example 1, except that:
the reactive monomer isobornyl methacrylate (IBOA) in which the monofunctional acrylate was replaced with the monofunctional acrylate reactive monomer lauric acrylate. But the resulting glue was not resistant to the electrolyte.
Comparative example 2
An insulating protective adhesive, which is substantially the same as the insulating protective adhesive of example 2 and is prepared by the preparation method of example 2, except that:
the difunctional acrylate tricyclodecane dimethanol diacrylate is replaced by the active monomer trimethylolpropane tri-methylol triacrylate of polyfunctional acrylate. However, the compatibility of trimethylolpropane triacrylate itself, which is an active monomer of multifunctional acrylate, with polybutadiene acrylate is not very good, and thus the electrolyte cannot be tolerated.
Examples
The performance test is carried out after the insulation protective adhesive prepared in the above examples and comparative examples is subjected to screen printing, and the method comprises the following steps:
viscosity: the viscosity at 25 ℃ is tested according to the standard GB/T22314-2008 viscosity test method for plastic epoxy resins.
Specific gravity: and (3) testing at 25 ℃ according to a density determination method of standard GB/T15223-.
Hardness: 23 +/-2 ℃, and measuring indentation hardness (Shore hardness) by using a durometer according to the standard GB/T2411-2008 plastic and hard rubber.
Hundred grids: according to the test of the GB/T9286-1998 national Standard for the test of marking test of paint films of paints and varnishes, the film thickness is 150-.
Acid and alkali resistance: the glue is coated on the surface of the aluminum sheet, the thickness of the glue is controlled to be 100-200 mu m, and OK is obtained if the aluminum sheet is soaked in various acids and alkalis without falling off or wrinkling.
Electrolyte resistance: the aluminum sheet is coated with glue with the thickness controlled at 100-.
Breakdown voltage: and in a standard GB/T1408.1-2006 test for industrial frequency short-time electrical strength of insulating materials, coating the surface of an aluminum sheet with glue, wherein the thickness of the glue is controlled to be 150-.
Wear resistance: in part 2 of the standard GBT 12967.2-2008 aluminum and aluminum alloy anodic oxide film detection method, a wheel type abrasion tester is used for measuring the abrasion resistance and the abrasion resistance coefficient of the anodic oxide film, the load is 1000g, the friction medium CS-17 is used, and the abrasion loss is less than 20 percent after 2000 times of operation, namely OK.
The test results were as follows:
TABLE 1 Performance test results
Figure BDA0001271544400000081
Figure BDA0001271544400000091
Note: "-" indicates: since the data is not important, no testing or comparison is performed;
"NG" means: not OK, fail the test or satisfy the use.
From the above results, it can be seen that the insulating protective adhesive of embodiments 1-2 of the present invention has excellent electrolyte tolerance, good insulating property, good adhesion, and good wear resistance, and can be used for insulating and isolating protection of the surface of the power battery aluminum shell instead of insulating paper. The glue of comparative examples 1-2 was less effective.
The technical features of the embodiments described above may be arbitrarily combined, and for the sake of brevity, all possible combinations of the technical features in the embodiments described above are not described, but should be considered as being within the scope of the present specification as long as there is no contradiction between the combinations of the technical features.
The above-mentioned embodiments only express several embodiments of the present invention, and the description thereof is more specific and detailed, but not construed as limiting the scope of the invention. It should be noted that, for a person skilled in the art, several variations and modifications can be made without departing from the inventive concept, which falls within the scope of the present invention. Therefore, the protection scope of the present patent shall be subject to the appended claims.

Claims (6)

1. The insulation protective adhesive is characterized by being mainly prepared from the following raw materials in parts by weight:
Figure FDA0002513505220000011
the oligomer is polybutadiene acrylate;
the active monomers are isobornyl methacrylate and tricyclodecane dimethanol diacrylate;
the photoinitiator is selected from: at least one of alpha-hydroxyketone derivatives, benzoyl formate, acylphosphine oxides, benzophenones and derivatives thereof.
2. The insulation protective paste according to claim 1, wherein the auxiliary agent is at least one of an adhesion promoter, a defoaming agent, and a leveling agent.
3. The adhesive according to claim 2, wherein the adhesion promoter is selected from the group consisting of: at least one of gamma-glycidoxypropyltrimethoxysilane, gamma-methacryloxypropyltrimethoxysilane, gamma-methacryloxypropyltriethoxysilane, and a polyfunctional thiol compound;
the defoaming agent is a silicone defoaming agent;
the leveling agent is an organic silicon leveling agent.
4. The method for preparing the insulation protection adhesive according to any one of claims 1 to 3, characterized by comprising the steps of:
preheating: preheating the oligomer;
and (3) hot mixing: keeping the preheating temperature, adding the active monomer, and completely dissolving the oligomer in the active monomer to obtain a mixed glue solution;
mixing: stopping heating, adding the photoinitiator and the auxiliary agent, and stirring uniformly under the condition of residual heat to obtain the high-performance ultraviolet curing coating.
5. The method for preparing insulation protective adhesive according to claim 4, wherein in the preheating step, the oligomer is heated to 50-70 ℃ for preheating.
6. Use of the insulating protective adhesive according to any one of claims 1 to 3 on the surface of an aluminum casing of a power battery.
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Citations (1)

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US5045386A (en) * 1989-02-01 1991-09-03 Minnesota Mining And Manufacturing Company Pressure-sensitive film composite having improved adhesion to plasticized vinyl substrates

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