CN114045136A - Flame-retardant bonding material capable of being cured in magnetic field and preparation method thereof - Google Patents

Flame-retardant bonding material capable of being cured in magnetic field and preparation method thereof Download PDF

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Publication number
CN114045136A
CN114045136A CN202111347756.XA CN202111347756A CN114045136A CN 114045136 A CN114045136 A CN 114045136A CN 202111347756 A CN202111347756 A CN 202111347756A CN 114045136 A CN114045136 A CN 114045136A
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magnetic field
flame
parts
retardant
preparation
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CN202111347756.XA
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Inventor
闫善涛
陈田安
王建斌
徐有志
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Yantai Darbond Technology Co Ltd
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Yantai Darbond Technology 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
    • C09J163/00—Adhesives based on epoxy resins; Adhesives based on derivatives of epoxy resins
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J3/00—Processes of treating or compounding macromolecular substances
    • C08J3/24—Crosslinking, e.g. vulcanising, of macromolecules
    • C08J3/246—Intercrosslinking of at least two polymers
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J3/00—Processes of treating or compounding macromolecular substances
    • C08J3/28—Treatment by wave energy or particle radiation
    • 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
    • C09J11/04—Non-macromolecular additives inorganic
    • 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
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J2363/00—Characterised by the use of epoxy resins; Derivatives of epoxy resins
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J2463/00—Characterised by the use of epoxy resins; Derivatives of epoxy resins
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00—Use of inorganic substances as compounding ingredients
    • C08K3/02—Elements
    • C08K3/08—Metals
    • C08K2003/0856—Iron
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00—Use of inorganic substances as compounding ingredients
    • C08K3/02—Elements
    • C08K3/08—Metals
    • C08K2003/0893—Zinc
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00—Use of inorganic substances as compounding ingredients
    • C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
    • C08K3/20—Oxides; Hydroxides
    • C08K3/22—Oxides; Hydroxides of metals
    • C08K2003/2227—Oxides; Hydroxides of metals of aluminium
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K2201/00—Specific properties of additives
    • C08K2201/011—Nanostructured additives
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00—Use of inorganic substances as compounding ingredients
    • C08K3/02—Elements
    • C08K3/08—Metals
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K5/00—Use of organic ingredients
    • C08K5/16—Nitrogen-containing compounds
    • C08K5/34—Heterocyclic compounds having nitrogen in the ring
    • C08K5/3467—Heterocyclic compounds having nitrogen in the ring having more than two nitrogen atoms in the ring
    • C08K5/3477—Six-membered rings
    • C08K5/3492—Triazines
    • C08K5/34928—Salts
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2201/00—Properties
    • C08L2201/02—Flame or fire retardant/resistant
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2201/00—Properties
    • C08L2201/22—Halogen free composition

Abstract

The invention relates to a magnetic field curable flame-retardant bonding material and a preparation method thereof, wherein the magnetic field curable flame-retardant bonding material is prepared from the following raw materials in parts by mass: 25-40 parts of epoxy resin, 8-13 parts of a toughening agent, 3-6 parts of metal nanoparticles, 0.4-0.6 part of black pigment, 40-55 parts of a filler and 4-6 parts of a curing agent. The bonding material prepared by the invention has the advantages of magnetic field curing, high curing speed, good flame retardant property and the like, is suitable for structural bonding of novel materials with various flame retardant property requirements, and effectively increases the safety and reliability of products.

Description

Flame-retardant bonding material capable of being cured in magnetic field and preparation method thereof
Technical Field
The invention relates to a magnetic field curable flame-retardant bonding material and a preparation method thereof, belonging to the field of adhesives.
Background
The so-called strategic emerging industry is an important force leading to the development of future economic society. The most popular 5G, consumer electronics, new energy automobiles and rail transit are strategic emerging industries. The 5G industry accelerates explosive development, and is embodied in unmanned aerial vehicles, head-mounted displays, robots, vehicle-mounted units and the like. The development of these techniques requires support by the adhesive material. The adhesive material has the characteristics of good adhesive force, good electrical insulation performance, light weight and the like, and can improve the functionality of the product.
Most of the currently marketed adhesive materials are in a heat curing mode, have the problem of damaging heat-sensitive materials, do not have good flame retardant property and have poor safety. The performance requirements brought by the development of product technology cannot be met.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provide the magnetic field curable flame-retardant bonding material and the preparation method thereof.
The technical scheme for solving the technical problems is as follows: a flame-retardant adhesive material capable of being cured by a magnetic field and a preparation method thereof are disclosed:
the weight portion of the material is as follows: 25-40 parts of epoxy resin, 8-13 parts of toughening agent and 3-6 parts of metal nano particles are sequentially put into a stirring kettle, a high-speed dispersion machine is used, the rotating speed is set to 2000RPM, stirring is carried out for 0.5-1 hour, then 0.4-0.6 part of black pigment, 40-55 parts of filler and 4-6 parts of curing agent are sequentially put into the stirring kettle, the rotating speed is set to 40RPM under the condition of vacuumizing, and stirring is carried out for 3-4 hours, so that the flame-retardant bonding material capable of being cured by the magnetic field is prepared.
The invention has the beneficial effects that: the flame-retardant bonding material prepared by the invention has the characteristic of magnetic field curing, the curing speed and the bonding force of the flame-retardant bonding material can be comparable to those of similar products cured by heating, and the bonding and fixing of various heat-sensitive materials are met. The flame retardant property is good, the risk of burning caused by overload of the miniaturized component is effectively prevented, and the safety and the reliability are improved.
On the basis of the technical scheme, the invention is further improved as follows.
Further, the epoxy resin is one or a mixture of two of EPLC-827, EPLC-828 and EPLC-818S which are produced by Shanghai New complexing Material Co.
The epoxy resin has the advantages of being high in reaction activity, good in bonding performance, low in total chlorine content and the like. The adhesive can react quickly in the curing process of the adhesive material, and has better adhesive property and environmental protection property after curing.
Further, the toughening agent is one or a mixture of two of FORTEGRA 100, FORTEGRA 202 produced by Dow USA or MX-125, MX-154 produced by Nippon Kogyo.
The further scheme has the beneficial effects that after the bonding material is cured, the toughening agent forms uniformly dispersed flexible molecular chain segments in a curing system, so that the bonding material has higher toughness and high bonding performance.
Further, the metal nanoparticles are manganese, zinc and iron composite metal nanoparticles with the particle size of 40-60 nm, which are produced by Xuzhou Jie Innovative materials science and technology Limited.
The metal nano particles are composed of manganese, zinc and iron composite metal nano particles, and after the metal nano particles pass through a magnetic field, when electromagnetic energy passes through the metal nano particles, heat can be released, and a system is activated to carry out molecular crosslinking curing reaction.
Further, the filler is a mixture of melamine cyanurate with the particle size of 1-4 microns and aluminum hydroxide with the particle size of 8-14 microns, which are produced by Hongtai flame retardant materials Limited of Dongguan city, and the preferable mixture ratio is 1: 2.
the further scheme has the beneficial effects that the melamine cyanurate is a nitrogen-containing halogen-free environment-friendly organic flame retardant, and has the characteristics of low smoke, low toxicity, easy dispersion, good flame retardant effect and the like; the aluminum hydroxide belongs to an inorganic flame retardant, is flame-retardant by releasing combined water, has the characteristics of good environmental protection, no smoke, no toxicity and the like, and is favorable for a system to have better flame-retardant effect by mixing the aluminum hydroxide and the water in a certain proportion.
Further, the curing agent is one or a mixture of two of FXR-1061 and FXR-1081 produced by Fuji chemical industries Co., Ltd, and MY-24 and MY-H produced by Koshikaki Kaisha.
The further scheme has the beneficial effects that the curing agent has good compatibility with epoxy resin, is easy to mix and disperse uniformly, and has the characteristics of low-temperature rapid curing and good storage stability.
Detailed Description
The principles and features of this invention are described below in conjunction with examples which are set forth to illustrate, but are not to be construed to limit the scope of the invention.
Example 1
The weight portion of the material is as follows: the flame-retardant adhesive material is prepared by sequentially putting 400g of epoxy resin EPLC-818S, 10080 g of toughening agent FORTEGRA and 60g of metal nanoparticles into a stirring kettle, setting the rotating speed to 2000RPM by using a high-speed dispersion machine, stirring for 1 hour, then sequentially putting 4g of black pigment, 150g of melamine cyanurate, 250g of aluminum hydroxide and FXR-108160 g of curing agent into the stirring kettle, setting the rotating speed to 40RPM under the condition of vacuumizing, and stirring for 4 hours.
Example 2
The weight portion of the material is as follows: sequentially putting epoxy resin EPLC-827110 g, epoxy resin EPLC-818S 200g, toughening agent MX-154100 g and metal nano particles 40g into a stirring kettle, using a high-speed dispersion machine, setting the rotating speed at 2000RPM, stirring for 1 hour, sequentially putting black pigment 4g, melamine cyanurate 250g, aluminum hydroxide 250g, curing agent FXR-106120 g and curing agent MY-2430 g into the stirring kettle, setting the rotating speed at 40RPM under the condition of vacuum pumping, and stirring for 4 hours to obtain the flame-retardant bonding material.
Example 3
The weight portion of the material is as follows: sequentially putting 250g of epoxy resin EPLC-818S, 202130 g of flexibilizer FORTEGRA and 50g of metal nanoparticles into a stirring kettle, using a high-speed dispersion machine, setting the rotating speed to 2000RPM, stirring for 1 hour, then sequentially putting 4g of black pigment, 175g of melamine cyanurate, 350g of aluminum hydroxide, FXR-108125 g of curing agent and MY-2420 g of curing agent into the stirring kettle, setting the rotating speed to 40RPM under the condition of vacuumizing, and stirring for 4 hours to obtain the flame-retardant bonding material.
Example 4
The weight portion of the material is as follows: sequentially putting epoxy resin EPLC-827100 g, epoxy resin EPLC-828150 g, toughening agent FORTEGRA 20280 g, toughening agent MX-12550 g and metal nanoparticles 30g into a stirring kettle, using a high-speed dispersion machine, setting the rotating speed to 2000RPM, stirring for 1 hour, sequentially putting black pigment 6g, melamine cyanurate 183g, aluminum hydroxide 367g and curing agent MY-H40 g into the stirring kettle, setting the rotating speed to 40RPM under the vacuum condition, and stirring for 4 hours to obtain the flame-retardant bonding material.
Comparative example 1
The weight portion of the material is as follows: putting 400g of epoxy resin EPLC-818S and 10080 g of toughening agent FORTEGRA into a stirring kettle in sequence, setting the rotating speed to 2000RPM by using a high-speed dispersion machine, when stirring for 1, putting 4g of black pigment, 150g of melamine cyanurate, 250g of aluminum hydroxide and FXR-108160 g of curing agent into the stirring kettle in sequence, setting the rotating speed to 40RPM under the condition of vacuumizing, and stirring for 4 hours to obtain the flame-retardant bonding material.
Comparative example 2
The weight portion of the material is as follows: sequentially putting 250g of epoxy resin EPLC-818S, 202130 g of flexibilizer FORTEGRA and 50g of metal nanoparticles into a stirring kettle, stirring for 1 hour at a set rotating speed of 2000RPM by using a high-speed dispersion machine, sequentially putting 4g of black pigment, 520g of aluminum hydroxide, 108130 g of curing agent FXR and 2420 g of curing agent MY into the stirring kettle, setting a rotating speed of 40RPM under a vacuum-pumping condition, and stirring for 4 hours to obtain the flame-retardant bonding material.
Comparative example 3
The weight portion of the material is as follows: sequentially putting epoxy resin EPLC-827100 g, epoxy resin EPLC-828150 g, toughening agent FORTEGRA 20280 g, toughening agent MX-12550 g and metal nanoparticles 30g into a stirring kettle, using a high-speed dispersion machine, setting the rotating speed to 2000RPM, stirring for 1 hour, sequentially putting black pigment 6g, melamine cyanurate 550g and curing agent MY-H40 g into the stirring kettle, setting the rotating speed to 40RPM under the vacuum condition, and stirring for 4 hours to obtain the flame-retardant bonding material.
Specific test examples
The epoxy resin adhesive materials of the above examples 1 to 4 of the present invention and comparative examples 1 to 3 were tested for their performance by the following tests. Wherein the magnetic field curable properties are characterized by the degree of cure; fast cure performance is characterized by the passage of a constant electromagnetic field time; the cohesive properties are characterized by shear strength; flame retardant performance is characterized by the burn time.
Test example 1 test of magnetic field-curable Properties
Using an SBV type electromagnet with the magnetic field intensity of 1.9T, taking 5-10 mg of a sample, placing for 20min to finish the curing process, and measuring the curing degree by using DSC (differential scanning calorimetry), wherein the unit percentage (%) is obtained. Test example 2 quick curability test
The magnet was left for a period of time in minutes (Min) in an SBV type magnet of magnetic field strength 1.9T when the degree of cure reached 95% as measured by DSC (differential scanning calorimetry).
Test example 3 adhesion Performance test
An electrothermal blowing drying box with the set temperature of 90 ℃ and an SBV-type electromagnet with the magnetic field intensity of 1.9T are respectively used for completing the solidification process of a sample in an aluminum sheet-to-aluminum sheet lapping mode, and a universal testing machine is used for testing the shear strength in unit megapascal (MPa).
Test example 4 flame retardancy test
The burning time after leaving the flame was measured in seconds(s) per UL94 horizontal vertical burning test method using a UL94 horizontal vertical burning tester.
The test results are shown in table 1 below.
Figure BDA0003354846290000051
Figure BDA0003354846290000061
TABLE 1 comparative test results of test performances of samples prepared in examples 1 to 4 and samples of comparative examples 1 to 3
As can be seen from the data in Table 1, the epoxy resin adhesive material prepared by the invention can rapidly complete the whole curing process in a magnetic field, has good adhesive force and basically consistent shear strength with the thermal curing process. Compared with single flame-retardant filler, the composite flame-retardant filler selected by the invention has obviously excellent flame-retardant performance, is suitable for structural bonding of novel materials with various flame-retardant performance requirements, and effectively increases the safety and reliability of products.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents, improvements and the like that fall within the spirit and principle of the present invention are intended to be included therein.

Claims (6)

1. The flame-retardant bonding material capable of being cured by a magnetic field and the preparation method thereof are characterized by comprising the following steps:
the weight portion of the material is as follows: 25-40 parts of epoxy resin, 8-13 parts of toughening agent and 3-6 parts of metal nano particles are sequentially put into a stirring kettle, a high-speed dispersion machine is used, the rotating speed is set to 2000RPM, stirring is carried out for 0.5-1 hour, then 0.4-0.6 part of black pigment, 40-55 parts of filler and 4-6 parts of curing agent are sequentially put into the stirring kettle, the rotating speed is set to 40RPM under the condition of vacuumizing, and stirring is carried out for 3-4 hours, so that the flame-retardant bonding material capable of being cured by the magnetic field is prepared.
2. The magnetic field curable flame retardant adhesive material and the preparation method thereof according to claim 1, wherein the epoxy resin is one or a mixture of two of EPLC-827, EPLC-828 and EPLC-818S manufactured by Shanghai New Complex Material Ltd.
3. The magnetic field curable flame retardant adhesive material and the preparation method thereof according to claim 1, wherein the toughening agent is one or a mixture of two of FORTEGRA 100, FORTEGRA 202 produced by Dow USA or MX-125, MX-154 produced by Kokko Japan.
4. The magnetic field curable flame retardant adhesive material and the preparation method thereof according to claim 1, wherein the metal nanoparticles are manganese, zinc, iron composite metal nanoparticles produced by Xuzhou Jie Innovation materials science and technology Limited.
5. The magnetic field curable flame-retardant adhesive material and the preparation method thereof according to claim 1, wherein the filler is a mixture of melamine cyanurate and aluminum hydroxide, which are produced by Hongtai flame-retardant materials Limited of Dongguan city, and the preferred mixture ratio is 1: 2.
6. the magnetic field-curable flame-retardant adhesive material according to claim 1, wherein the curing agent is one or a mixture of FXR-1061 and FXR-1081 available from Fuji chemical industries, Ltd., or MY-24 and MY-H available from Kumamoto chemical industries, Ltd.
CN202111347756.XA 2021-11-15 2021-11-15 Flame-retardant bonding material capable of being cured in magnetic field and preparation method thereof Pending CN114045136A (en)

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Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105924729A (en) * 2016-05-30 2016-09-07 李岩 Flame-retardant cable material
CN109096972A (en) * 2018-09-29 2018-12-28 沈阳建筑大学 A kind of magnetic heat molten type epoxyn and its application
CN111471280A (en) * 2020-05-13 2020-07-31 沈阳理工大学 Microwave irradiation and magnetic heat induction curing resin and preparation method thereof

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105924729A (en) * 2016-05-30 2016-09-07 李岩 Flame-retardant cable material
CN109096972A (en) * 2018-09-29 2018-12-28 沈阳建筑大学 A kind of magnetic heat molten type epoxyn and its application
CN111471280A (en) * 2020-05-13 2020-07-31 沈阳理工大学 Microwave irradiation and magnetic heat induction curing resin and preparation method thereof

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