CN112961634B - Elastic wave glue and preparation method and application thereof - Google Patents
Elastic wave glue and preparation method and application thereof Download PDFInfo
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- CN112961634B CN112961634B CN202110163862.6A CN202110163862A CN112961634B CN 112961634 B CN112961634 B CN 112961634B CN 202110163862 A CN202110163862 A CN 202110163862A CN 112961634 B CN112961634 B CN 112961634B
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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
- C09J11/04—Non-macromolecular additives inorganic
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- H—ELECTRICITY
- H04—ELECTRIC COMMUNICATION TECHNIQUE
- H04R—LOUDSPEAKERS, MICROPHONES, GRAMOPHONE PICK-UPS OR LIKE ACOUSTIC ELECTROMECHANICAL TRANSDUCERS; DEAF-AID SETS; PUBLIC ADDRESS SYSTEMS
- H04R31/00—Apparatus or processes specially adapted for the manufacture of transducers or diaphragms therefor
- H04R31/003—Apparatus or processes specially adapted for the manufacture of transducers or diaphragms therefor for diaphragms or their outer suspension
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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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- 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
- C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend
- C08L2205/035—Polymer mixtures characterised by other features containing three or more polymers in a blend containing four or more polymers in a blend
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Abstract
The invention relates to a glue solution, in particular to an elastic wave glue and a preparation method and application thereof. The preparation raw materials of the elastic wave adhesive comprise, by weight, 5-14 parts of an epoxy resin emulsifier, 30-50 parts of modified epoxy resin, 0.1-1 part of a curing accelerator, 8-15 parts of an epoxy curing agent and 20-35 parts of water. The elastic wave glue is transparent aqueous emulsion, has excellent dispersibility, wettability, hardness and toughness, is easy to coat on the surface of a nylon base material when in use, has excellent coating uniformity, and has excellent sound transmission effect when being applied to a vibrating diaphragm material of a loudspeaker and the like.
Description
Technical Field
The invention relates to a glue solution, in particular to an elastic wave glue and a preparation method and application thereof.
Background
The elastic wave is prepared by coating elastic wave glue on cloth and is one of important elements of the loudspeaker, the elastic wave glue is used for the elastic wave of the loudspeaker on a disc frame, and the connection between a paper edge and the disc frame can be used for sealing between a washer and the disc frame. The elastic wave glue is prepared from some resins, the traditional elastic wave glue is a glue solution prepared from phenolic resin, but the glue solution needs methanol and other harmful substances, and has certain harm to human bodies. And the elastic wave glue prepared from the phenolic resin glue solution has poor high and low temperature resistance and poor elasticity, and easily generates fatigue under the vibration action of a high-power loudspeaker to cause sound distortion. The flatness of the elastic waves prepared by coating the conventional elastic wave glue on cloth is poor, and the performance of a loudspeaker is also influenced.
Disclosure of Invention
In order to solve the technical problems, the first aspect of the invention provides an elastic wave glue, and the raw materials for preparing the elastic wave glue comprise, by weight, 5-14 parts of an epoxy resin emulsifier, 30-50 parts of a modified epoxy resin, 0.1-1 part of a curing accelerator, 8-15 parts of an epoxy curing agent and 20-35 parts of water.
In a preferred embodiment of the present invention, the modified epoxy resin includes a water-based rubber-modified epoxy resin.
As a preferable technical scheme, the raw materials for preparing the aqueous rubber modified epoxy resin comprise epoxy resin E-44, aqueous epoxy resin emulsion, liquid rubber, graphene oxide dispersion liquid, liquid rubber and deionized water.
In a preferred embodiment of the present invention, the modified epoxy resin further comprises an aqueous resin for an elastic wave glue.
In a preferred embodiment of the present invention, the graphene oxide in the graphene oxide dispersion liquid has 2 to 6 layers.
As a preferable technical solution of the present invention, the modified epoxy resin further includes an acrylic modified epoxy resin.
As a preferable technical scheme of the invention, the raw materials for preparing the epoxy resin emulsifier comprise epoxy resin E-44, an emulsifier and an initiator.
As a preferable technical solution of the present invention, the raw material for preparing the elastic wave rubber further comprises at least one of a lubricant, a dispersant and a wetting agent.
The second aspect of the invention provides a preparation method of an elastic wave glue, which comprises the following steps:
(1) Uniformly stirring a curing accelerator, an epoxy curing agent and 1/2 of water by weight to obtain a solution A;
(2) Stirring the preparation raw materials of the modified epoxy resin, the epoxy resin emulsifier and the rest of the elasto-sol at 40-55 ℃ for 30-40min to obtain a solution B;
(3) And (3) mixing and stirring the solution A and the solution B uniformly at room temperature to obtain the elastic wave glue.
The third aspect of the invention provides application of the elastic wave glue for preparing elastic waves.
The invention has the following beneficial effects:
1. the elastic wave glue prepared by using the modified epoxy resin has excellent toughness;
2. the epoxy resin is emulsified into a microemulsion state, and the prepared elastic wave glue has excellent toughness and stability;
3. the elastic wave glue is transparent aqueous emulsion, has excellent dispersibility and wettability, is easy to coat on the surface of a nylon base material when in use, has excellent coating uniformity, and has excellent sound transmission effect when being applied to a vibrating diaphragm material of a loudspeaker and the like;
4. the elastic wave rubber has excellent hardness, toughness and aging resistance, does not deform after being used for a long time and vibrated for many times, and has excellent durability;
5. the elastic wave glue can be quickly cured on a base material.
Drawings
Fig. 1 is a graph showing the displacement (fatigue deflection resistance) of the shockwave sample 1 in example 3, in which the abscissa represents the test distance and the ordinate represents the test tensile force.
Detailed Description
The invention will be further understood by reference to the following detailed description of preferred embodiments of the invention and the examples included therein. 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. To the extent that a definition of a particular term disclosed in the prior art is inconsistent with any definition provided in the present disclosure, the definition of the term provided in the present disclosure controls.
As used herein, a feature that is not limited to a single plural form is also intended to include plural forms of the feature unless the context clearly indicates otherwise. It will also be understood that the term "prepared from …" as used herein is synonymous with "comprising," including, "comprising," "has," "contains," and/or "contains," when used in this specification means the recited composition, step, method, article, or apparatus, but does not preclude the presence or addition of one or more other compositions, steps, methods, articles, or apparatuses. Furthermore, the use of "preferred," "preferably," "more preferred," etc., when describing embodiments of the present invention, is meant to refer to embodiments of the invention that may provide certain benefits, under certain circumstances. However, other embodiments may be preferred, under the same or other circumstances. In addition, the recitation of one or more preferred embodiments does not imply that other embodiments are not useful, nor is it intended to exclude other embodiments from the scope of the invention.
The invention provides a elasto-wave adhesive, which is prepared from the following raw materials, by weight, 5-14 parts of an epoxy resin emulsifier, 30-50 parts of a modified epoxy resin, 0.1-1 part of a curing accelerator, 8-15 parts of an epoxy curing agent and 20-35 parts of water.
In a preferred embodiment, the raw materials for preparing the elastic wave glue comprise, by weight, 7-10 parts of an epoxy resin emulsifier, 35-40 parts of a modified epoxy resin, 0.3-0.5 part of a curing accelerator, 10-14 parts of an epoxy curing agent and 25-30 parts of water.
In a preferred embodiment, the raw materials for preparing the elastic wave rubber comprise, by weight, 8 parts of epoxy resin emulsifier, 38 parts of modified epoxy resin, 0.4 part of curing accelerator, 13 parts of epoxy curing agent and 27 parts of water.
In one embodiment, the raw materials for preparing the elastic wave rubber further comprise at least one of a lubricant, a dispersant and a wetting agent.
In one embodiment, the raw materials for preparing the elastic wave rubber further comprise a lubricant, a dispersant and a wetting agent; wherein the weight ratio of the lubricant to the dispersant to the wetting agent is (1.2-1.5): (1.6-2): 1; further preferably, the weight ratio of the lubricant to the dispersant to the wetting agent is 1.3:1.8:1.
in one embodiment, the total weight of the lubricant, the dispersant and the wetting agent is 0.8-1.5% of the weight of the raw materials for preparing the elastic wave rubber; further preferably, the total weight of the lubricant, the dispersant and the wetting agent is 1.2% of the weight of the raw materials for preparing the elastorubber.
Epoxy resin emulsifier
In one embodiment, the raw materials for preparing the epoxy resin emulsifier comprise epoxy resin E-44, an emulsifier and an initiator.
In one embodiment, the epoxy resin emulsifier is prepared from 10-14 parts by weight of epoxy resin E-44, 50-60 parts by weight of emulsifier and 0.4-0.8 part by weight of initiator.
In a preferred embodiment, the raw materials for preparing the epoxy resin emulsifier comprise, by weight, 12 parts of epoxy resin E-44, 55 parts of emulsifier and 0.6 part of initiator.
In one embodiment, the epoxy resin E-44 is from Sandeli chemical industries, inc. of Jiangsu.
In one embodiment, the emulsifier is an ethylene oxide condensate.
In a preferred embodiment, the ethylene oxide condensate has a hydroxyl number of from 26 to 63mKOH/g; further preferably, the ethylene oxide condensate has a hydroxyl value of 34 to 42mKOH/g.
In one embodiment, the ethylene oxide condensate is PEG-3000.
The initiator is not particularly limited, and examples thereof include azobisisobutyronitrile, potassium persulfate, diacyl peroxide and the like.
In one embodiment, the initiator is potassium persulfate.
In one embodiment, the epoxy resin emulsifier is prepared by the method comprising: uniformly mixing the epoxy resin E-44 and the emulsifier, heating the system to 85-100 ℃, adding the initiator, and reacting for 3-4h at 160-180 ℃ to obtain the epoxy resin emulsifier.
In a preferred embodiment, the epoxy resin emulsifier is prepared by the following steps: and (3) uniformly mixing the oxygen resin E-44 and the emulsifier, heating the system to 95 ℃, adding an initiator, and reacting for 3.5 hours at 170 ℃ to obtain the epoxy resin emulsifier.
The applicant finds that the use of the epoxy resin emulsifier in the system of the present invention allows the elastic wave prepared from the bulk elastic wave glue to have good flatness and the loudspeaker prepared by using the elastic wave to have good sound quality. It is possible that the epoxy resin emulsifier prepared in the present invention is in a micro-emulsion state, so that the substances in the present invention are compatible with wettability.
Modified epoxy resin
In one embodiment, the modified epoxy resin comprises a waterborne rubber modified epoxy resin.
In one embodiment, the raw materials for preparing the aqueous rubber modified epoxy resin comprise epoxy resin E-44, an aqueous epoxy resin emulsion, liquid rubber, a graphene oxide dispersion, liquid rubber and deionized water.
In one embodiment, the raw materials for preparing the aqueous rubber modified epoxy resin comprise, by weight, 70-90 parts of epoxy resin E-44, 16-20 parts of aqueous epoxy resin emulsion, 12-15 parts of liquid rubber, 8-13 parts of graphene oxide dispersion liquid, and 58-65 parts of deionized water.
In a preferred embodiment, the raw materials for preparing the aqueous rubber modified epoxy resin comprise, by weight, 80 parts of epoxy resin E-44, 18 parts of aqueous epoxy resin emulsion, 13 parts of liquid rubber, 10 parts of graphene oxide dispersion and 62 parts of deionized water.
In one embodiment, the step of preparing the aqueous rubber-modified epoxy resin comprises:
s1: reacting epoxy resin E-44 with liquid rubber at 150-170 ℃ for 2-4h to obtain a mixed material A;
s2: and adding the aqueous epoxy resin emulsion into the mixed material A, reacting at 50-70 ℃ for 30-50min, then adding deionized water and the graphene oxide dispersion liquid, and carrying out ultrasonic reaction for 3-3.5h to obtain the aqueous rubber modified epoxy resin.
In one embodiment, the aqueous epoxy resin emulsion has an epoxy equivalent weight of 300 to 350g/eq; more preferably, the epoxy equivalent of the aqueous epoxy resin emulsion is 330g/eq.
In one embodiment, the aqueous epoxy resin emulsion is a DOW aqueous epoxy resin DER 916.
In one embodiment, the liquid rubber is selected from at least one of an acrylate-based liquid rubber, a diene-based liquid rubber, a liquid nitrile rubber; further preferably, the liquid rubber is a diene-based liquid rubber.
In one embodiment, the diene-based liquid rubber is a butadiene-based liquid rubber and/or a pentadiene-based rubber; further preferably, the diene-based liquid rubber is a butadiene-based rubber.
In a preferred embodiment, the butadiene-based rubber is a hydroxyl-terminated liquid polybutadiene rubber.
In one embodiment, the hydroxyl-terminated liquid polybutadiene rubber is purchased from Jingjiang city, tokyo, korea, inc.
The applicant has found that the addition of the aqueous rubber modified epoxy resin to the system of the present invention can increase the fatigue resistance and water resistance of the elastomer. On one hand, the defect of poor toughness of the epoxy resin E-44 is improved probably due to the mutual synergistic action of the liquid rubber and the epoxy resin E-44, and on the other hand, the crosslinking density of the system is increased probably due to the fact that certain crosslinking action is generated between the hydroxyl group, the carboxyl group and the like on the surface of the graphene oxide in the graphene oxide dispersion liquid and the epoxy resin matrix in the system.
In one embodiment, the modified epoxy resin further comprises an aqueous resin for an elastomer gel.
In one embodiment, the weight of the waterborne resin for the elastic wave glue is 20-30% of the weight of the modified epoxy resin; more preferably, the weight of the aqueous resin for the elastic wave glue is 25% of the weight of the modified epoxy resin.
In one embodiment, the aqueous elastomer resin is an aqueous elastomer resin prepared by the Kyoho Seisakusho, wherein the aqueous elastomer resin contains a silicon group and a long-chain group.
In one embodiment, the graphene oxide in the graphene oxide dispersion liquid is 2 to 6 layers.
In a preferred embodiment, the graphene oxide in the graphene oxide dispersion liquid is 3 to 5 layers; more preferably, the graphene oxide in the graphene oxide dispersion liquid is 4 layers.
In one embodiment, the graphene oxide dispersion is purchased from Jiangsu Xifeng nanomaterial science and technology Co.
The applicant invents that the high-temperature and low-temperature denaturation resistance of the system can be improved by adding the water-based resin for the elastic wave glue into the system, and the high-temperature and low-temperature denaturation resistance of the elastic wave glue can be further improved by selecting the multi-layer graphene oxide dispersion liquid. Probably because the long-chain groups contained in the aqueous resin for the elasto-rubber can be mutually and synergistically acted with the aqueous rubber modified epoxy resin through the interpenetration effect of the graphene oxide with a multilayer structure in the preparation process.
In one embodiment, the modified epoxy resin further comprises an acrylic modified epoxy resin.
In one embodiment, the weight of the acrylic modified epoxy resin is 25-32% of the weight of the modified epoxy resin; more preferably, the weight of the acrylic modified epoxy resin is 28% of the weight of the modified epoxy resin.
In one embodiment, the acrylic-modified epoxy resin is available from Rongzhong chemical Co., ltd, dongguan.
The applicant adds the acrylic acid modified epoxy resin into the system to aim at the adhesion of the elastic wave glue on the base material, but unexpectedly finds that the addition of the acrylic acid modified epoxy resin into the system can increase the tone quality of the loudspeaker, probably because the acrylic acid group in the acrylic acid modified epoxy resin is changed to be more uniformly adhered on the base material in the interaction period with other long chain groups in the system.
Curing accelerator
The curing accelerator is an imidazole accelerator; examples of the imidazole-based accelerator include 2-methylimidazole, 2-ethylimidazole, 2-phenylimidazole, 1-cyanoethyl-2-ethyl-4-methylimidazole, and 1-cyanoethyl-2-phenylimidazole.
In a preferred embodiment, the imidazole-based accelerator is 1-cyanoethyl-2-ethyl-4-methylimidazole.
In one embodiment, the 1-cyanoethyl-2-ethyl-4-methylimidazole is 2E4MZ-CN made in four countries of japan.
Epoxy curing agent
In one embodiment, the epoxy curing agent is not particularly limited; examples of the curing agent include DOW Dow aqueous epoxy curing agent D.E.H.805, DOW Dow aqueous epoxy curing agent D.E.H.804, vandaisea chemical aqueous epoxy curing agent HDH6127, vandaisea chemical aqueous epoxy curing agent HDH6119, and the like.
In one embodiment, the epoxy curing agent is a DOW waterborne epoxy curing agent d.e.h.804.
Water (I)
The water is not particularly limited and may be distilled water, deionized water, pure water, or the like.
In one embodiment, the water is deionized water.
Lubricant agent
The lubricant is not limited, and lubricants suitable for aqueous epoxy resin systems are all suitable for the system; examples of the lubricant include magnesium stearate, zinc stearate, stearic acid, and stearamide.
In one embodiment, the lubricant is stearic acid (CAS number: 57-11-4).
Dispersing agent
The dispersant is not limited, and lubricants suitable for aqueous epoxy resin systems are all suitable for the system; examples of the dispersant include Disperbyk-180, tamol 901, orotan 963, BYK-192, BYK-190, and Hydropalat 100.
In one embodiment, the dispersant is Orotan 963.
Wetting agent
The wetting agent is not limited, and the wetting agents suitable for the waterborne epoxy resin system are all suitable for the system; as the wetting agent, teGo270, BYK-348, BYK-346, DOW-NP-100, BYK-349, BYK346 and the like can be exemplified.
In one embodiment, the wetting agent is BYK-349.
The second aspect of the invention provides a preparation method of an elastic wave glue, which comprises the following steps:
(1) Uniformly stirring a curing accelerator, an epoxy curing agent and 1/2 of water by weight to obtain a solution A;
(2) Stirring the modified epoxy resin, the epoxy resin emulsifier and the rest raw materials for preparing the elasto-wave glue at 40-55 ℃ for 30-40min to obtain a solution B;
(3) And (3) mixing and stirring the solution A and the solution B uniformly at room temperature to obtain the elastic wave glue.
In a preferred embodiment, the preparation method of the elastic wave glue comprises the following steps:
(1) Uniformly stirring a curing accelerator, an epoxy curing agent and 1/2 of water by weight to obtain a solution A;
(2) Stirring the preparation raw materials of the modified epoxy resin, the epoxy resin emulsifier and the rest of the elasto-sol for 35min at 50 ℃ to obtain a solution B;
(3) And mixing and stirring the solution A and the solution B uniformly at room temperature to obtain the elastic wave rubber.
In one embodiment, the stirring speed in step (2) is 1800 to 2300rpm/min; further preferably, the stirring speed in the step (2) is 2000rpm/min.
The third aspect of the invention provides application of the damper adhesive for preparing the damper.
Several specific examples of the present invention are given below, but the present invention is not limited by the examples.
In addition, the starting materials in the present invention are all commercially available unless otherwise specified.
Examples
Example 1
The embodiment 1 of the invention specifically provides an elastic wave glue, and the preparation raw materials of the elastic wave glue comprise, by weight, 7 parts of an epoxy resin emulsifier, 35 parts of a modified epoxy resin, 0.3 part of a curing accelerator, 10 parts of an epoxy curing agent and 25 parts of water;
the raw materials for preparing the elastic wave rubber also comprise a lubricant, a dispersant and a wetting agent; wherein the weight ratio of the lubricant to the dispersant to the wetting agent is 1.2:1.6:1; the total weight of the lubricant, the dispersant and the wetting agent is 0.8 percent of the weight of the preparation raw material of the elasto-damping adhesive;
the preparation raw materials of the epoxy resin emulsifier comprise, by weight, 10 parts of epoxy resin E-44, 50 parts of emulsifier and 0.4 part of initiator; the emulsifier is an ethylene oxide condensate; the hydroxyl value of the ethylene oxide condensate is 34-42mKOH/g; the initiator is potassium persulfate;
the preparation method of the epoxy resin emulsifier comprises the following steps: uniformly mixing epoxy resin E-44 and an emulsifier, heating the system to 85 ℃, adding an initiator, and reacting for 4 hours at 160 ℃ to obtain an epoxy resin emulsifier;
the modified epoxy resin comprises a water-based rubber modified epoxy resin; the preparation raw materials of the waterborne rubber modified epoxy resin comprise, by weight, 70 parts of epoxy resin E-44, 16 parts of waterborne epoxy resin emulsion, 12 parts of liquid rubber, 8 parts of graphene oxide dispersion liquid and 58 parts of deionized water;
the preparation method of the waterborne rubber modified epoxy resin comprises the following steps:
s1: reacting epoxy resin E-44 with liquid rubber at 150 ℃ for 4h to obtain a mixed material A;
s2: adding a water-based epoxy resin emulsion into the mixed material A to react for 50min at 50 ℃, and then adding deionized water and graphene oxide dispersion liquid to perform ultrasonic reaction for 3h to obtain water-based rubber modified epoxy resin;
the epoxy equivalent of the waterborne epoxy resin emulsion is 330g/eq; the liquid rubber is diene liquid rubber; the diene liquid rubber is butadiene rubber; the butadiene rubber is hydroxyl-terminated liquid polybutadiene rubber; the modified epoxy resin also comprises an aqueous resin for elastic wave glue; the weight of the water-based resin for the elastic wave glue is 20% of that of the modified epoxy resin; the aqueous resin for the elastic wave glue is prepared by the science and technology company Limited of the fine and novel materials in Guangzhou city, wherein the aqueous resin for the elastic wave glue contains a silicon group and a long-chain group;
the graphene oxide in the graphene oxide dispersion liquid is 3 layers; the modified epoxy resin also comprises acrylic acid modified epoxy resin; the weight of the acrylic acid modified epoxy resin is 25 percent of that of the modified epoxy resin;
the curing accelerator is an imidazole accelerator; the imidazole accelerator is 1-cyanoethyl-2-ethyl-4-methylimidazole;
the water is deionized water;
the preparation method of the elastic wave glue comprises the following steps:
(1) Uniformly stirring a curing accelerator, an epoxy curing agent and 1/2 of water by weight to obtain a solution A;
(2) Stirring the preparation raw materials of the modified epoxy resin, the epoxy resin emulsifier and the rest of the elasto-sol for 40min at 40 ℃ to obtain a solution B;
(3) Mixing and stirring the solution A and the solution B uniformly at room temperature to obtain an elastic wave adhesive;
the stirring speed in the step (2) is 1800rpm/min.
The epoxy resin E-44 is from Sanzhihua chemical Co., ltd, jiangsu; the ethylene oxide condensate is PEG-3000; the waterborne epoxy resin emulsion is DOW waterborne epoxy resin DER 916; the hydroxyl-terminated liquid polybutadiene rubber is purchased from Jingjiang city, tong, high chemical industry Co., ltd; the graphene oxide dispersion liquid is purchased from Jiangsu Xiancheng nano material science and technology limited; the acrylic acid modified epoxy resin is purchased from Rongzhong chemical industry Co., ltd, dongguan city; the 1-cyanoethyl-2-ethyl-4-methylimidazole is 2E4MZ-CN which is formed by four nations of Japan; the epoxy curing agent is DOW Dow waterborne epoxy curing agent D.E.H.804; the lubricant is stearic acid (CAS number: 57-11-4); the dispersant is Orotan 963; the wetting agent is BYK-349.
Example 2
Embodiment 2 of the invention specifically provides an elastic wave adhesive, and the preparation raw materials of the elastic wave adhesive comprise, by weight, 10 parts of an epoxy resin emulsifier, 40 parts of a modified epoxy resin, 0.5 part of a curing accelerator, 14 parts of an epoxy curing agent and 30 parts of water; the raw materials for preparing the elastic wave rubber also comprise a lubricant, a dispersant and a wetting agent; wherein the weight ratio of the lubricant to the dispersant to the wetting agent is 1.5:2:1; the total weight of the lubricant, the dispersant and the wetting agent is 1.5 percent of the weight of the preparation raw material of the elasto-damping adhesive;
the preparation raw materials of the epoxy resin emulsifier comprise, by weight, 14 parts of epoxy resin E-44, 60 parts of emulsifier and 0.8 part of initiator; the emulsifier is an ethylene oxide condensate; the hydroxyl value of the ethylene oxide condensate is 34-42mKOH/g; the initiator is potassium persulfate;
the preparation method of the epoxy resin emulsifier comprises the following steps: uniformly mixing epoxy resin E-44 and an emulsifier, heating the system to 100 ℃, adding an initiator, and reacting at 180 ℃ for 3 hours to obtain an epoxy resin emulsifier;
the modified epoxy resin comprises a water-based rubber modified epoxy resin; the preparation raw materials of the waterborne rubber modified epoxy resin comprise, by weight, 90 parts of epoxy resin E-44, 20 parts of waterborne epoxy resin emulsion, 15 parts of liquid rubber, 13 parts of graphene oxide dispersion liquid and 65 parts of deionized water;
the preparation method of the waterborne rubber modified epoxy resin comprises the following steps:
s1: reacting the epoxy resin E-44 with liquid rubber at 170 ℃ for 2h to prepare a mixed material A;
s2: adding aqueous epoxy resin emulsion into the mixed material A, reacting for 30min at 70 ℃, then adding deionized water and graphene oxide dispersion liquid, and carrying out ultrasonic reaction for 3.5h to obtain aqueous rubber modified epoxy resin;
the epoxy equivalent of the aqueous epoxy resin emulsion is 330g/eq.
The liquid rubber is diene liquid rubber; the diene liquid rubber is butadiene rubber; the butadiene rubber is hydroxyl-terminated liquid polybutadiene rubber; the modified epoxy resin also comprises an aqueous resin for elastic wave glue; the weight of the water-based resin for the elastic wave glue is 30% of that of the modified epoxy resin; the aqueous resin for the elastic wave glue is prepared by the science and technology company Limited of the fine and novel materials in Guangzhou city, wherein the aqueous resin for the elastic wave glue contains a silicon group and a long-chain group;
the graphene oxide in the graphene oxide dispersion liquid is 5 layers; the modified epoxy resin also comprises acrylic acid modified epoxy resin; the weight of the acrylic acid modified epoxy resin is 32 percent of that of the modified epoxy resin;
the curing accelerator is an imidazole accelerator; the imidazole accelerator is 1-cyanoethyl-2-ethyl-4-methylimidazole;
the water is deionized water;
the preparation method of the elastic wave glue comprises the following steps:
(1) Uniformly stirring a curing accelerator, an epoxy curing agent and 1/2 of water by weight to obtain a solution A;
(2) Stirring the preparation raw materials of the modified epoxy resin, the epoxy resin emulsifier and the rest of the elasto-wave glue for 30min at 55 ℃ to obtain a solution B;
(3) Mixing and stirring the solution A and the solution B uniformly at room temperature to obtain an elastic wave adhesive;
the stirring speed in the step (2) is 2300rpm/min.
The epoxy resin E-44 is from Sanzhihua chemical Co., ltd, jiangsu; the ethylene oxide condensate is PEG-3000; the waterborne epoxy resin emulsion is DOW waterborne epoxy resin DER 916; the hydroxyl-terminated liquid polybutadiene rubber is purchased from Jingjiang city, tokyo high chemical engineering Co., ltd; the graphene oxide dispersion liquid is purchased from Jiangsu Xiancheng nano material science and technology limited; the acrylic acid modified epoxy resin is purchased from Rongzhong chemical industry Co., ltd, dongguan city; the 1-cyanoethyl-2-ethyl-4-methylimidazole is 2E4MZ-CN which is formed by four nations of Japan; the epoxy curing agent is DOW Dow waterborne epoxy curing agent D.E.H.804; the lubricant is stearic acid (CAS number: 57-11-4); the dispersant is Orotan 963; the wetting agent is BYK-349.
Example 3
Embodiment 3 of the invention specifically provides an elastic wave adhesive, and the preparation raw materials of the elastic wave adhesive comprise, by weight, 8 parts of an epoxy resin emulsifier, 38 parts of a modified epoxy resin, 0.4 part of a curing accelerator, 13 parts of an epoxy curing agent and 27 parts of water; the raw materials for preparing the elastic wave rubber also comprise a lubricant, a dispersant and a wetting agent; wherein the weight ratio of the lubricant to the dispersant to the wetting agent is 1.3:1.8:1; the total weight of the lubricant, the dispersant and the wetting agent is 1.2 percent of the weight of the preparation raw material of the elasto-sol;
the preparation raw materials of the epoxy resin emulsifier comprise, by weight, 12 parts of epoxy resin E-44, 55 parts of emulsifier and 0.6 part of initiator; the emulsifier is an ethylene oxide condensate; the hydroxyl value of the ethylene oxide condensate is 34-42mKOH/g; the initiator is potassium persulfate;
the preparation method of the epoxy resin emulsifier comprises the following steps: uniformly mixing the oxygen resin E-44 and the emulsifier, heating the system to 95 ℃, adding the initiator, and reacting for 3.5 hours at 170 ℃ to obtain the epoxy resin emulsifier;
the modified epoxy resin comprises a water-based rubber modified epoxy resin; the preparation raw materials of the waterborne rubber modified epoxy resin comprise, by weight, 80 parts of epoxy resin E-44, 18 parts of waterborne epoxy resin emulsion, 13 parts of liquid rubber, 10 parts of graphene oxide dispersion liquid and 62 parts of deionized water;
the preparation method of the waterborne rubber modified epoxy resin comprises the following steps:
s1: reacting epoxy resin E-44 with liquid rubber at 160 ℃ for 3h to obtain a mixed material A;
s2: adding aqueous epoxy resin emulsion into the mixed material A, reacting for 40min at 60 ℃, then adding deionized water and graphene oxide dispersion liquid, and carrying out ultrasonic reaction for 3.2h to obtain aqueous rubber modified epoxy resin;
the epoxy equivalent of the waterborne epoxy resin emulsion is 330g/eq; the liquid rubber is diene liquid rubber; the diene liquid rubber is butadiene rubber; the butadiene rubber is hydroxyl-terminated liquid polybutadiene rubber;
the modified epoxy resin also comprises an aqueous resin for elastic wave glue; the weight of the water-based resin for the elastic wave glue is 25% of that of the modified epoxy resin; the aqueous resin for the elastic wave glue is prepared by the science and technology company Limited of the fine and novel materials in Guangzhou city, wherein the aqueous resin for the elastic wave glue contains a silicon group and a long-chain group; the graphene oxide in the graphene oxide dispersion liquid is 4 layers; the modified epoxy resin also comprises acrylic acid modified epoxy resin; the weight of the acrylic acid modified epoxy resin is 28 percent of that of the modified epoxy resin;
the curing accelerator is an imidazole accelerator; the imidazole accelerator is 1-cyanoethyl-2-ethyl-4-methylimidazole.
The water is deionized water;
the preparation method of the elastic wave glue comprises the following steps:
(1) Uniformly stirring a curing accelerator, an epoxy curing agent and 1/2 of water by weight to obtain a solution A;
(2) Stirring the preparation raw materials of the modified epoxy resin, the epoxy resin emulsifier and the rest of the elasto-wave glue for 35min at 50 ℃ to obtain a solution B;
(3) Mixing and stirring the solution A and the solution B uniformly at room temperature to obtain an elastic wave adhesive;
the stirring speed in the step (2) is 2000rpm/min.
The epoxy resin E-44 is from Jiangsu Sanmuhua chemical Co., ltd; the ethylene oxide condensate is PEG-3000; the waterborne epoxy resin emulsion is DOW waterborne epoxy resin DER 916; the hydroxyl-terminated liquid polybutadiene rubber is purchased from Jingjiang city, tong, high chemical industry Co., ltd; the graphene oxide dispersion liquid is purchased from Jiangsu Xiancheng nano material science and technology limited; the acrylic acid modified epoxy resin is purchased from Rongzhong chemical industry Co., ltd, dongguan city; the 1-cyanoethyl-2-ethyl-4-methylimidazole is 2E4MZ-CN which is formed by four nations of Japan; the epoxy curing agent is DOW Dow waterborne epoxy curing agent D.E.H.804; the lubricant is stearic acid (CAS number: 57-11-4); the dispersant is Orotan 963; the wetting agent is BYK-349.
Example 4
Embodiment 4 of the present invention specifically provides an elasto-rubber, and the specific implementation manner is the same as that in embodiment 3, except that hydroxyl-terminated liquid butyl rubber is used instead of hydroxyl-terminated liquid polybutadiene rubber.
Example 5
Example 5 of the present invention specifically provides an elastomeric compound, which is the same as example 3 in the specific embodiment except that the epoxy resin is modified with anhydrous rubber.
Example 6
Embodiment 6 of the present invention specifically provides an elastic wave glue, and a specific implementation manner thereof is the same as that in embodiment 3, except that the graphene oxide in the graphene oxide dispersion liquid is 1 layer.
Example 7
Embodiment 7 of the present invention specifically provides an elastomeric wave glue, and the specific implementation manner thereof is the same as that in embodiment 3, except that no acrylic acid modified epoxy resin is used.
Example 8
Embodiment 8 of the invention specifically provides an elastic wave adhesive, and the preparation raw materials of the elastic wave adhesive comprise, by weight, epoxy resin E-448 parts, modified epoxy resin 38 parts, curing accelerator 0.4 part, epoxy curing agent 13 parts, and water 27 parts; the raw materials for preparing the elastic wave rubber also comprise a lubricant, a dispersant and a wetting agent; wherein the weight ratio of the lubricant to the dispersant to the wetting agent is 1.3:1.8:1; the total weight of the lubricant, the dispersant and the wetting agent is 1.2 percent of the weight of the preparation raw material of the elasto-sol;
the modified epoxy resin, the curing accelerator, the epoxy curing agent, the water, the lubricant, the dispersant and the wetting agent are the same as those in the embodiment 3;
the preparation method of the elastic wave glue comprises the following steps:
(1) Uniformly stirring a curing accelerator, an epoxy curing agent and 1/2 of water by weight to obtain a solution A;
(2) Stirring the preparation raw materials of the modified epoxy resin, the epoxy resin E44 and the rest of the elastic wave glue for 35min at 50 ℃ to obtain a solution B;
(3) Mixing and stirring the solution A and the solution B uniformly at room temperature to prepare the elastic wave glue;
the stirring speed in the step (2) is 2000rpm/min.
The epoxy resin E-44 is from Sandeli chemical industries, inc. of Jiangsu.
Performance testing
Preparation of damper sample-1: the example and the commercially available elastic wave glue are respectively coated on 20T double 36 cotton cloth with the coating thickness of 10 microns, the 20T double 36 cotton cloth coated with the elastic wave glue is dried at 115 ℃ for 4 hours, then the cotton cloth is placed into a mold and heated at 225 ℃ for 25min, and finally the elastic wave with the diameter of 11 cm and 7 lines is obtained through molding and cutting.
Preparation of damper sample-2: the examples and the commercially available elastic wave glue are respectively coated on 24T cotton cloth with the coating thickness of 10 microns, the 24T cotton cloth coated with the elastic wave glue is dried at 115 ℃ for 4 hours, then the 24T cotton cloth is placed in a mold and heated at 225 ℃ for 25min, and finally, the elastic wave glue is molded and cut to obtain 5-line elastic waves with the diameter of 8 cm.
Test examples 1 to 8:1. the method comprises the following steps of stability testing, 2 flatness testing, 3 fatigue resistance testing and 4 high and low temperature deflection testing.
1. And (3) stability testing:
1.1 equipment: displacement test system, 100 gram weight.
1.2 test method: taking the elastic wave sample-1 to fix the inner and outer edges of the elastic wave (10 samples are taken, each sample is tested for 10 times), adding a fixed 100 weights in the middle of the inner edge of the elastic wave sample-1, measuring the descending distance of the elastic wave sample-1 and the elastic wave sample after the weights are pressed down, and finally calculating the absolute displacement: absolute displacement = maximum descent distance-minimum descent distance, taking its average; the method for testing the stability of the damper sample-2 is the same as that of the damper sample-1.
2. And (3) flatness testing:
2.1 equipment: a plug gauge.
2.2 test methods: taking an elastic wave sample-1, naturally placing the product on a platform, measuring the maximum position of the edge of the product and the platform by using a plug gauge as flatness, measuring 10 samples, respectively measuring 10 times, and taking an average value.
The flatness of the damper sample-2 is tested in the same manner as the damper sample-1.
3. And (3) fatigue resistance test:
3.1 equipment: a displacement test system, a 50g weight and an up-and-down vibration system;
3.2 test method: initial measurement: taking an elastic wave sample-1 (5, testing for 5 times), fixing the inner edge and the outer edge of an elastic wave, adding a fixed 50-gram weight in the middle of the inner edge of the elastic wave sample-1, measuring the descending distance of the elastic wave sample-1 after the weight is pressed down, and taking the average initial displacement distance F1;
measuring after the up-down vibration system vibrates 50000 times: fixing the inner and outer edges of the elastic wave (5 elastic wave samples respectively), adding 50 fixed weights in the middle of the inner edge of the elastic wave, measuring the descending distance of the elastic wave after the weights are pressed down, and taking the displacement measurement value F2 after the weights vibrate up and down on average;
absolute displacement = F2-F1;
the method for testing the fatigue resistance of the elastic wave sample-2 is the same as that of the elastic wave sample-1.
4. High and low temperature deflection test:
4.1 equipment: high-low temperature experiment machine
4.2 test method: dividing 10 elastic wave samples-1 into 2 groups, and respectively testing the average initial displacement distance F (initial); then, the two sets of samples were left at 105 ℃ and-40 ℃ for 24 hours, respectively, and then the average displacement distance F (latter) was measured.
Displacement deviation = [ F (initial) -F (post) ]/F (initial) × 100%.
5. Displacement (fatigue deflection resistance):
5.1. equipment: tension tester
5.2. The test method comprises the following steps: the inner and outer diameters of the shockwave sample-1 (1 sample) in example 3 were fixed, the maximum force of pull-up and pull-down was inputted, and the force returned when the force reached the maximum. When the test is completed, see if the bullet wave returns to the origin.
5.3. Test values are: plus or minus 30N
The test results are shown in fig. 1: in the figure, the abscissa represents the test distance and the ordinate represents the test tensile force.
5.4. And (4) conclusion: through the power of 30N, make displacement test, the bullet ripples of playing can return to the original point completely.
The commercially available elastic wave rubber is used as a comparative example, and the stability test, the flatness test, the fatigue resistance test and the high and low temperature deflection test are carried out according to the same test method.
The test results are shown in Table 1
TABLE 1
The foregoing examples are merely illustrative and serve to explain some of the features of the method of the present invention. The appended claims are intended to claim as broad a scope as is contemplated, and the examples presented herein are merely illustrative of selected implementations in accordance with all possible combinations of examples. Accordingly, it is applicants' intention that the appended claims are not to be limited by the choice of examples illustrating features of the invention. Also, where numerical ranges are used in the claims, subranges therein are included, and variations in these ranges are also to be construed as possible being covered by the appended claims.
Claims (4)
1. The elastic wave glue is characterized in that the preparation raw materials of the elastic wave glue comprise, by weight, 5-14 parts of an epoxy resin emulsifier, 30-50 parts of a modified epoxy resin, 0.1-1 part of a curing accelerator, 8-15 parts of an epoxy curing agent and 20-35 parts of water; the raw materials for preparing the epoxy resin emulsifier comprise, by weight, 10-14 parts of epoxy resin E-44, 50-60 parts of emulsifier and 0.4-0.8 part of potassium persulfate; the modified epoxy resin comprises a water-based rubber modified epoxy resin; the preparation raw materials of the waterborne rubber modified epoxy resin comprise, by weight, 70-90 parts of epoxy resin E-44, 16-20 parts of waterborne epoxy resin emulsion, 12-15 parts of liquid rubber, 8-13 parts of graphene oxide dispersion liquid and 58-65 parts of deionized water; the liquid rubber is hydroxyl-terminated liquid polybutadiene rubber; the graphene oxide in the graphene oxide dispersion liquid is 2-6 layers; the modified epoxy resin also comprises acrylic acid modified epoxy resin; the weight of the acrylic acid modified epoxy resin is 25-32% of the weight of the modified epoxy resin.
2. The ebonite according to claim 1, wherein the raw materials for preparing the ebonite further comprise at least one of a lubricant, a dispersant, and a wetting agent.
3. A method of preparing an elasto-rubber according to any one of claims 1-2, characterized in that it comprises the following steps:
(1) Uniformly stirring a curing accelerator, an epoxy curing agent and 1/2 of water by weight to obtain a solution A;
(2) Stirring the modified epoxy resin, the epoxy resin emulsifier and the rest raw materials for preparing the elasto-wave glue at 40-55 ℃ for 30-40min to obtain a solution B;
(3) And mixing and stirring the solution A and the solution B uniformly at room temperature to obtain the elastic wave rubber.
4. Use of an elastomer according to any of claims 1-2 for the preparation of an elastomer.
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| CN103596114A (en) * | 2012-08-16 | 2014-02-19 | 大原博 | Horn elastic wave and manufacturing method thereof |
| CN108251031A (en) * | 2017-12-29 | 2018-07-06 | 常州思宇知识产权运营有限公司 | A kind of stretch-proof type splicing adhesive |
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