CN109439252B - Epoxy resin sealant and preparation method and application thereof - Google Patents
Epoxy resin sealant and preparation method and application thereof Download PDFInfo
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- CN109439252B CN109439252B CN201811264609.4A CN201811264609A CN109439252B CN 109439252 B CN109439252 B CN 109439252B CN 201811264609 A CN201811264609 A CN 201811264609A CN 109439252 B CN109439252 B CN 109439252B
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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
- C09J163/00—Adhesives based on epoxy resins; Adhesives based on derivatives of epoxy resins
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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
- 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
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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
- C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
- C09J11/08—Macromolecular additives
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/02—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group
- C08L2205/025—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group containing two or more polymers of the same hierarchy C08L, and differing only in parameters such as density, comonomer content, molecular weight, structure
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- Epoxy Resins (AREA)
- Sealing Battery Cases Or Jackets (AREA)
Abstract
The invention discloses an epoxy resin sealant and a preparation method and application thereof. The sealant is composed of a component A and a component B, wherein the component A comprises the following components in parts by weight: 75-80 parts of bisphenol F type epoxy resin, 7-10 parts of bisphenol A type epoxy resin, 1-1.2 parts of silane coupling agent and 10-15 parts of diluent; the component B comprises the following components in parts by weight: 30-35 parts of curing agent, 25-30 parts of accelerator I, 20-25 parts of accelerator II and 12-17 parts of solvent. According to the invention, through optimizing the components and the proportion of the sealant, the bonding property and the acid corrosion resistance of the epoxy resin sealant can be effectively improved, so that the epoxy resin sealant is suitable for sealing a lead-acid storage battery cover made of polyphenyl ether.
Description
Technical Field
The invention relates to the technical field of epoxy resin sealants, in particular to an epoxy resin sealant and a preparation method and application thereof.
Background
Polyphenylene Oxide (PPO) is one of five general engineering plastics in the world, and has the advantages of high rigidity, high heat resistance, flame retardancy, high strength, excellent electrical property and the like. In addition, PPO also has the advantages of wear resistance, no toxicity, pollution resistance and the like. The dielectric constant and dielectric loss of PPO are one of the smallest varieties in engineering plastics, are hardly influenced by temperature and humidity, and can be used in the fields of low, medium and high-frequency electric fields. The use of PPO in lead acid batteries is therefore of increasing interest.
Molded articles and extruded articles of polyphenylene ether and modified polyphenylene ether are generally bonded by using a solvent-based adhesive or an adhesive solution, and impurities and contamination on the surface must be completely removed in the bonding process, as in the case of other plastics; in social environments with high environmental requirements, solvent-based adhesives are increasingly restricted.
Lead-acid storage battery manufacturers in the current market are different in form, but relatively few reports are reported about epoxy middle cover sealant for a storage battery made of PPO materials, and the main reason is that the lead-acid storage battery made of PPO materials is higher in bonding difficulty and stricter in sealing requirement compared with the traditional ABS materials. If the epoxy resin storage battery middle cover glue which is commonly used in the market at present is adopted as the epoxy middle cover sealant for the storage battery made of PPO materials, the problem of low bonding strength can occur, the bonding strength is only about 5MPa, and the epoxy resin storage battery middle cover sealant is used for sealing a storage battery groove cover and at least has certain guarantee on the quality of a storage battery product when reaching more than 6 MPa. Therefore, there is a need for a sealant having good adhesion and being used for sealing a cover of a polyphenylene ether lead-acid battery.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provide the epoxy resin sealant, the preparation method and the application thereof, so that the bonding property and the acid corrosion resistance of the epoxy resin sealant are improved, and the epoxy resin sealant is suitable for sealing a lead-acid storage battery cover made of polyphenyl ether.
In order to achieve the purpose, the technical scheme adopted by the invention is as follows:
the epoxy resin sealant consists of a component A and a component B, wherein the component A comprises the following components in parts by weight: 75-80 parts of bisphenol F type epoxy resin, 7-10 parts of bisphenol A type epoxy resin, 1-1.2 parts of silane coupling agent and 10-15 parts of diluent; the component B comprises the following components in parts by weight: 30-35 parts of curing agent, 25-30 parts of accelerator I, 20-25 parts of accelerator II and 12-17 parts of solvent.
The invention selects bisphenol F type epoxy resin as a main body, has low viscosity, better wettability to PPO surface and better corrosion resistance after curing, effectively improves the bonding property and acid corrosion resistance of the epoxy resin sealant by optimizing the components and the proportion of the sealant, and is suitable for sealing the lead-acid storage battery tank cover made of polyphenyl ether.
As a preferred embodiment of the epoxy resin sealant of the present invention, the curing agent is polyether amine.
As a preferred embodiment of the epoxy resin sealant, the accelerator I is 2, 4, 6-tris (dimethylaminomethyl) phenol.
In a preferred embodiment of the epoxy resin sealant of the present invention, the accelerator II is 2, 4, 6-tris (dimethylaminomethyl) phenolate.
As a preferred embodiment of the epoxy resin sealant, the sealant consists of a component A and a component B, wherein the component A comprises the following components in parts by weight: 79.5 parts of bisphenol F type epoxy resin, 8.5 parts of bisphenol A type epoxy resin, 1 part of silane coupling agent and 11 parts of diluent; the component B comprises the following components in parts by weight: 30 parts of curing agent, 28 parts of accelerator I, 25 parts of accelerator II and 17 parts of solvent.
As a preferred embodiment of the epoxy resin sealant, the silane coupling agent is KH560, the diluent is a bifunctional epoxy diluent, and the solvent is benzyl alcohol.
The invention selects the difunctional epoxy diluent, which not only reduces the viscosity and is easy for process operation, but also reduces the influence of the diluent on the bonding performance to the maximum extent; the addition of the coupling agent KH-560 helps to improve the bonding property of the epoxy resin sealant and PPO; the curing agent adopts polyether amine, so that the cured product keeps equivalent toughness, and the bonding property of PPO is ensured to the maximum extent; in the curing system, the di-tertiary amine accelerator 2, 4, 6-tri (dimethylaminomethyl) phenol and 2, 4, 6-tri (dimethylaminomethyl) phenate are matched for use, so that the curing speed is increased, the production efficiency is ensured, the operation time at room temperature is kept, and the production requirement is met.
The preparation method of the epoxy resin sealant comprises the following steps:
(1) preparation of component A: firstly, adding bisphenol F type epoxy resin and bisphenol A type epoxy resin into a stirring kettle, uniformly stirring, then adding a diluent and a silane coupling agent, dispersing for 15-20 min at the rotating speed of 1000-1200 r/min, and then carrying out vacuum defoaming at the vacuum degree of-0.098-0.1 MPa for 1-1.5 h to obtain a component A;
(2) preparation of the component B: and adding the curing agent, the accelerator I, the accelerator II and the solvent into stirring equipment in proportion, and uniformly stirring to obtain a component B.
The invention also provides the application of the epoxy resin sealant for sealing the lead-acid storage battery cover made of polyphenyl ether.
As a preferable embodiment of the application, the component A and the component B are added into a mixing container according to the weight ratio of 100: 25-30 and are uniformly stirred, then the cover of the storage battery tank is filled with glue, and the storage battery tank is cured for 1 hour at 70 ℃.
Compared with the prior art, the invention has the beneficial effects that:
the invention selects bisphenol F type epoxy resin as a main body, compounds bisphenol A type epoxy resin, has low viscosity, has better wettability on the PPO surface and better corrosion resistance after curing, effectively improves the bonding property and acid corrosion resistance of the epoxy resin sealant by optimizing the components and the proportion of the sealant, and is suitable for sealing the lead-acid storage battery tank cover made of polyphenyl ether.
Detailed Description
To better illustrate the objects, aspects and advantages of the present invention, the present invention will be further described with reference to specific examples. It will be understood by those skilled in the art that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
In the examples, the experimental methods used were all conventional methods unless otherwise specified, and the materials, reagents and the like used were commercially available without otherwise specified.
Example 1
As an embodiment of the epoxy resin sealant, the epoxy resin sealant of this embodiment includes a component a and a component B, where the component a includes the following components in parts by weight: 79.5 parts of bisphenol F type epoxy resin, 8.5 parts of bisphenol A type epoxy resin, KH-5601 parts of silane coupling agent and 11 parts of bifunctional epoxy diluent; the component B comprises the following components in parts by weight: 30 parts of polyether amine, 28 parts of 2, 4, 6-tri (dimethylaminomethyl) phenol (DMP-30), 25 parts of 2, 4, 6-tri (dimethylaminomethyl) phenolate (DMP-30 salt) and 17 parts of benzyl alcohol.
The preparation method of the epoxy resin sealant comprises the following steps:
(1) preparation of component A: firstly, adding bisphenol F type epoxy resin and bisphenol A type epoxy resin into a stirring kettle, uniformly stirring, then adding a bifunctional epoxy diluent and KH-560, dispersing for 15-20 min at the rotating speed of 1000-1200 r/min, and then carrying out vacuum deaeration for 1-1.5 h under the vacuum degree of-0.098-0.1 MPa to obtain a component A;
(2) preparation of the component B: adding the polyether amine, the DMP-30 salt and the benzyl alcohol into stirring equipment in proportion, and uniformly stirring to obtain a component B;
(3) and adding the component A and the component B into a mixing container according to the weight ratio of 100:25, uniformly stirring, filling glue into a storage battery tank cover, and curing for 1 hour at 70 ℃.
The test results of the sealant of this example are shown in table 1:
TABLE 1
The results in Table 1 show that the PPO shear strength of the sealant in the embodiment reaches more than 8MPa, and the sealant has good adhesion property and acid corrosion resistance, and is suitable for sealing the lead-acid storage battery cover made of polyphenyl ether.
Example 2
As an embodiment of the epoxy resin sealant, the epoxy resin sealant of this embodiment includes a component a and a component B, where the component a includes the following components in parts by weight: 78 parts of bisphenol F type epoxy resin, 8 parts of bisphenol A type epoxy resin, KH-5601.1 parts of silane coupling agent and 12.9 parts of bifunctional epoxy diluent; the component B comprises the following components in parts by weight: 35 parts of polyether amine, 25 parts of DMP-3025 parts of DMP-30 salt and 15 parts of benzyl alcohol.
The preparation method of the epoxy resin sealant comprises the following steps:
(1) preparation of component A: firstly, adding bisphenol F type epoxy resin and bisphenol A type epoxy resin into a stirring kettle, uniformly stirring, then adding a bifunctional epoxy diluent and KH-560, dispersing for 15-20 min at the rotating speed of 1000-1200 r/min, and then carrying out vacuum deaeration for 1-1.5 h under the vacuum degree of-0.098-0.1 MPa to obtain a component A;
(2) preparation of the component B: adding the polyether amine, the DMP-30 salt and the benzyl alcohol into stirring equipment in proportion, and uniformly stirring to obtain a component B;
(3) and adding the component A and the component B into a mixing container according to the weight ratio of 100:25, uniformly stirring, filling glue into a storage battery tank cover, and curing for 1 hour at 70 ℃.
The test results of the sealant of this example are shown in table 2:
TABLE 2
Example 3
As an embodiment of the epoxy resin sealant, the epoxy resin sealant of this embodiment includes a component a and a component B, where the component a includes the following components in parts by weight: 77 parts of bisphenol F epoxy resin, 7 parts of bisphenol A epoxy resin, KH-5601 parts of silane coupling agent and 15 parts of bifunctional epoxy diluent; the component B comprises the following components in parts by weight: 33 parts of polyether amine, 20 parts of DMP-3030 parts of DMP-30 salt and 17 parts of benzyl alcohol.
The preparation method of the epoxy resin sealant comprises the following steps:
(1) preparation of component A: firstly, adding bisphenol F type epoxy resin and bisphenol A type epoxy resin into a stirring kettle, uniformly stirring, then adding a bifunctional epoxy diluent and KH-560, dispersing for 15-20 min at the rotating speed of 1000-1200 r/min, and then carrying out vacuum deaeration for 1-1.5 h under the vacuum degree of-0.098-0.1 MPa to obtain a component A;
(2) preparation of the component B: adding the polyether amine, the DMP-30 salt and the benzyl alcohol into stirring equipment in proportion, and uniformly stirring to obtain a component B;
(3) and adding the component A and the component B into a mixing container according to the weight ratio of 100:28, uniformly stirring, filling the storage battery tank cover with glue, and curing for 1 hour at 70 ℃.
The test results of the sealant of this example are shown in table 3:
TABLE 3
Example 4
As an embodiment of the epoxy resin sealant, the epoxy resin sealant of this embodiment includes a component a and a component B, where the component a includes the following components in parts by weight: 80 parts of bisphenol F type epoxy resin, 9 parts of bisphenol A type epoxy resin, KH-5601 parts of silane coupling agent and 10 parts of bifunctional epoxy diluent; the component B comprises the following components in parts by weight: 34 parts of polyether amine, 3028 parts of DMP-3028, 22 parts of DMP-30 salt and 16 parts of benzyl alcohol.
The preparation method of the epoxy resin sealant comprises the following steps:
(1) preparation of component A: firstly, adding bisphenol F type epoxy resin and bisphenol A type epoxy resin into a stirring kettle, uniformly stirring, then adding a bifunctional epoxy diluent and KH-560, dispersing for 15-20 min at the rotating speed of 1000-1200 r/min, and then carrying out vacuum deaeration for 1-1.5 h under the vacuum degree of-0.098-0.1 MPa to obtain a component A;
(2) preparation of the component B: adding the polyether amine, the DMP-30 salt and the benzyl alcohol into stirring equipment in proportion, and uniformly stirring to obtain a component B;
(3) and adding the component A and the component B into a mixing container according to the weight ratio of 100:30, uniformly stirring, filling glue into a storage battery tank cover, and curing for 1 hour at 70 ℃.
The test results of the sealant of this example are shown in table 4:
TABLE 4
Comparative example 1
The epoxy resin sealant comprises a component A and a component B, wherein the component A comprises the following components in parts by weight: 79.5 parts of bisphenol F type epoxy resin, 8.5 parts of bisphenol A type epoxy resin, KH-5601 parts of silane coupling agent and 11 parts of bifunctional epoxy diluent; the component B comprises the following components in parts by weight: 30 parts of alicyclic amine curing agent, DMP-3028 parts, 2, 25 parts of dimethylbenzylamine and 17 parts of benzyl alcohol.
The preparation method of the epoxy resin sealant comprises the following steps:
(1) preparation of component A: firstly, adding bisphenol F type epoxy resin and bisphenol A type epoxy resin into a stirring kettle, uniformly stirring, then adding a bifunctional epoxy diluent and KH-560, dispersing for 15-20 min at the rotating speed of 1000-1200 r/min, and then carrying out vacuum deaeration for 1-1.5 h under the vacuum degree of-0.098-0.1 MPa to obtain a component A;
(2) preparation of the component B: adding the alicyclic amine curing agent, DMP-30, dimethylbenzylamine and benzyl alcohol into stirring equipment in proportion, and uniformly stirring to obtain a component B;
(3) and adding the component A and the component B into a mixing container according to the weight ratio of 100:25, uniformly stirring, filling glue into a storage battery tank cover, and curing for 1 hour at 70 ℃.
The test results for the sealant of this comparative example are shown in table 5:
TABLE 5
Comparative example 2
The epoxy resin sealant comprises a component A and a component B, wherein the component A comprises the following components in parts by weight: 79.5 parts of bisphenol F type epoxy resin, 8.5 parts of bisphenol A type epoxy resin, KH-5601 parts of silane coupling agent and 11 parts of bifunctional epoxy diluent; the component B comprises the following components in parts by weight: 40 parts of polyether amine, 25 parts of DMP-3020 parts of DMP-30 salt and 15 parts of benzyl alcohol.
The preparation method of the epoxy resin sealant comprises the following steps:
(1) preparation of component A: firstly, adding bisphenol F type epoxy resin and bisphenol A type epoxy resin into a stirring kettle, uniformly stirring, then adding a bifunctional epoxy diluent and KH-560, dispersing for 15-20 min at a high speed, and then defoaming in vacuum at a vacuum degree of-0.098-0.1 MPa for 1-1.5 h to obtain a component A;
(2) preparation of the component B: adding the polyether amine, the DMP-30 salt and the benzyl alcohol into stirring equipment in proportion, and uniformly stirring to obtain a component B;
(3) and adding the component A and the component B into a mixing container according to the weight ratio of 100:25, uniformly stirring, filling glue into a storage battery tank cover, and curing for 1 hour at 70 ℃. The test results for the sealant of this comparative example are shown in table 6:
TABLE 6
As shown in the results in tables 1-6, compared with the comparative example, the sealant disclosed by the invention has better bonding strength and acid corrosion resistance by optimizing the components and the content thereof, and is more suitable for sealing the lead-acid storage battery cover made of polyphenyl ether. According to the invention, bisphenol F epoxy resin is used as a main body, the viscosity is low, the PPO surface has good wettability, and the cured product has excellent corrosion resistance; the double-function diluent is selected, so that the viscosity is reduced, the process operation is easy, and the influence of the diluent on the bonding performance is reduced to the maximum extent; the addition of the coupling agent KH-560 helps to improve the bonding property of the epoxy resin sealant and PPO; the curing agent adopts polyether amine, so that the cured product keeps equivalent toughness, and the bonding property of PPO is ensured to the maximum extent; the dual-tertiary amine accelerator in the curing system is matched for use, so that the curing speed is improved, the production efficiency is ensured, the operation time at room temperature is kept, and the production requirement is met. The components and the proportion of the sealant are optimized, so that the adhesive property and the acid corrosion resistance of the epoxy resin sealant are effectively improved, and the epoxy resin sealant is suitable for sealing a lead-acid storage battery cover made of polyphenyl ether.
Finally, it should be noted that the above embodiments are only used for illustrating the technical solutions of the present invention and not for limiting the protection scope of the present invention, and although the present invention is described in detail with reference to the preferred embodiments, it should be understood by those skilled in the art that modifications or equivalent substitutions can be made on the technical solutions of the present invention without departing from the spirit and scope of the technical solutions of the present invention.
Claims (6)
1. The epoxy resin sealant is characterized by consisting of a component A and a component B, wherein the component A comprises the following components in parts by weight: 75-80 parts of bisphenol F type epoxy resin, 7-10 parts of bisphenol A type epoxy resin, 1-1.2 parts of silane coupling agent and 10-15 parts of diluent; the component B comprises the following components in parts by weight: 30-35 parts of a curing agent, 25-30 parts of an accelerator I, 20-25 parts of an accelerator II and 12-17 parts of a solvent; the curing agent is polyether amine; the accelerator I is 2, 4, 6-tris (dimethylaminomethyl) phenol; the accelerant II is 2, 4, 6-tris (dimethylaminomethyl) phenolate.
2. The epoxy resin sealant according to claim 1, which is composed of a component A and a component B, wherein the component A comprises the following components in parts by weight: 79.5 parts of bisphenol F type epoxy resin, 8.5 parts of bisphenol A type epoxy resin, 1 part of silane coupling agent and 11 parts of diluent; the component B comprises the following components in parts by weight: 30 parts of curing agent, 28 parts of accelerator I, 25 parts of accelerator II and 17 parts of solvent.
3. The epoxy resin sealant according to claim 1, wherein the silane coupling agent is KH560, the diluent is a difunctional epoxy diluent, and the solvent is benzyl alcohol.
4. The method for preparing the epoxy resin sealant according to any one of claims 1 to 3, characterized by comprising the steps of:
(1) preparation of component A: firstly, adding bisphenol F type epoxy resin and bisphenol A type epoxy resin into a stirring kettle, uniformly stirring, then adding a diluent and a silane coupling agent, dispersing for 15-20 min at the rotating speed of 1000-1200 r/min, and then carrying out vacuum defoaming at the vacuum degree of-0.098-0.1 MPa for 1-1.5 h to obtain a component A;
(2) preparation of the component B: and adding the curing agent, the accelerator I, the accelerator II and the solvent into stirring equipment in proportion, and uniformly stirring to obtain a component B.
5. Use of the epoxy resin sealant according to any one of claims 1 to 3 for sealing a cell cover of a polyphenylene ether lead-acid battery.
6. The use of the composition as claimed in claim 5, wherein the composition A and the composition B are added into a mixing container according to a weight ratio of 100: 25-30, uniformly stirred, and then the cover of the storage battery is filled with glue and cured for 1 hour at 70 ℃.
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| CN100480353C (en) * | 2007-01-29 | 2009-04-22 | 刘永祥 | Accumulator sealant |
| CN101525439B (en) * | 2008-12-31 | 2012-06-27 | 上海康达化工新材料股份有限公司 | Modified epoxide resin for structural adhesive of wind generating blades and preparation method thereof |
| CN101457133B (en) * | 2009-01-09 | 2012-05-30 | 宜兴市江南药用化工厂 | Lead accumulator epoxy resin sealant and preparation method thereof |
| US8741988B2 (en) * | 2010-06-15 | 2014-06-03 | Basf Se | Use of cyclic carbonates in epoxy resin compositions |
| KR101401640B1 (en) * | 2012-06-14 | 2014-06-02 | 주식회사 이피케미칼 | Epoxy resin composition containing silica and core-shell polymer particles |
| CN102925093A (en) * | 2012-11-27 | 2013-02-13 | 广州市泰为合成材料有限公司 | Lead-acid storage battery sealing gum |
| CN103725241B (en) * | 2014-01-16 | 2015-07-15 | 日邦树脂(无锡)有限公司 | Epoxy resin adhesive for encapsulating lead-acid storage battery and preparation method thereof |
| CN105176465B (en) * | 2015-10-13 | 2017-12-08 | 湖南全辰科技有限公司 | A kind of epoxy mortar and preparation method thereof |
| CN106281160B (en) * | 2016-08-08 | 2018-09-14 | 武汉拓路特铺技术工程有限公司 | A kind of normal temperature cure flexible epoxy adhesive and preparation method thereof |
| JP6964428B2 (en) * | 2017-03-31 | 2021-11-10 | ソマール株式会社 | Epoxy resin adhesive |
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