CN104845045A - Room-temperature curable epoxy resin based high damping material and preparation method thereof - Google Patents
Room-temperature curable epoxy resin based high damping material and preparation method thereof Download PDFInfo
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- CN104845045A CN104845045A CN201510216412.3A CN201510216412A CN104845045A CN 104845045 A CN104845045 A CN 104845045A CN 201510216412 A CN201510216412 A CN 201510216412A CN 104845045 A CN104845045 A CN 104845045A
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Abstract
The invention provides a room-temperature curable epoxy resin based high damping material and a preparation method thereof. The room-temperature curable epoxy resin based high damping material is mainly composed of a bisphenol A epoxy resin, a polyurethane modified epoxy resin, a silane coupling agent, a mixed amine curing agent and a curing accelerant as major components; liquid materials are divided into components A and B; the resins are heated at a constant temperature in an electric heating air-blast drying box firstly, thoroughly and evenly mixed, and then blended; the components are mixed independently in a mixing tank, stirred evenly by use of a stirrer, barreled in groups, and sealed, and therefore, the preparation of the room-temperature curable epoxy resin based high damping material is completed. The room-temperature curable epoxy resin based high damping material has the characteristics of high damping property, wide damping temperature range, long construction period, natural curing in a room-temperature environment and the like.
Description
[technical field]
The present invention relates to a kind of damping material and preparation method thereof, be specifically related to a kind of room temperature curing epoxy base high-damping material and preparation method thereof.
[background technology]
Known, the visco-elastic damping materials such as polymer are a kind of internal friction motion responses by molecule segment, dissipate in surrounding environment by encouraging the energy transformation of its vibration or sound wave to become heat energy, thus a kind of material of damped vibration and acoustic energy, it has very important effect in engineering vibration and noise reducing field, the noise level of some equipment directly or indirectly affects its state of the art, structure vibrated or acoustic wave excitation time, the in-fighting of directly related with effect of vibration and noise reduction is material, i.e. damping capacity, the parameter of exosyndrome material in-fighting size is dynamic properties parameter (the store elastic modulus E ' of material, loss Young's modulus E " and dissipation factor tan δ) and present temperature range and the frequency band of high in-fighting.The wherein loss Young's modulus E of material " and (or) dissipation factor tan δ is larger, present high loss Young's modulus E " and (or) the temperature range of dissipation factor tan δ is larger, frequency band is wider, and its effect of vibration and noise reduction is better.
The visco-elastic damping material of the current overwhelming majority is mainly with solid polymeric material, as body material made by rubber, elastomerics or resin, casting type, embedding type, coating-type relatively less, mostly be esters of acrylic acid, polyurethane kind and IPN (interpenetrating polymer networks) etc., general dissipation factor temperature range is narrower, and the highest loss factor is not high yet.Self-vulcanizing wide temperature zone high damping casting type material, is specially adapted to the position of the narrow regions vibratory noise process such as some gaps, corner.
Chinese patent, publication number is CN20061958707A, it discloses a kind of damp embedding glue of epoxy resin, for sealing and the slowing down vibration of electron device or unicircuit, main ingredient is rigidity epoxy and flexible epoxy, reactive thinner and liquid acrylonitrile butadiene rubber, has wider damping temperature range.
Chinese patent, publication number is CN101186803A, it discloses a kind of casting type epoxy resin base damping packaging material, industrialization encapsulation for electronic devices and components is produced, there is instantaneous high impact-resistance, be made up of bisphenol A epoxide resin, polyurethane-epoxy resin and flexible-epoxy etc., highest loss factor t an δ max >=0.5.
Chinese patent, publication number is CN103320073A, it discloses a kind of casting type epoxy resin base high-damping encapsulating compound, the industrialization encapsulation for electronic devices and components, parts is produced and is prevented plant and instrument because of external impacts, vibration and cause damage, the stability of raising equipment and reliability.Be made up of bisphenol A epoxide resin, polyurethane-epoxy resin, flexible-epoxy, reactive thinner, aliphatic amide, aliphatic cyclic amine, Versamid etc., highest loss factor t an δ max >=0.9.
Chinese patent, publication number is CN102093528A, it discloses a kind of mixed polyether-polyester polyurethane/epoxy damping composite preparation method, and the highest loss factor t an δ max drawn from curve is about 1.13.
Above patent not mentioned employing Amino Terminated polyether(ATPE) (or polyetheramine) solidifying agent, does not add restriction to the characteristic of each based epoxy resin yet, and the wide temperature range characteristic data of material is unknown, there is obvious otherness with the application.
United States Patent (USP), publication number is USP5331062, and it discloses a kind of polyurethane/epoxy resin IPN (interpenetrating polymer networks) acoustic damping material, it is modified version acoustic damping material, the maximum loss factor of 20 DEG C lower than 0.5.
Japanese Patent, publication number is JPS63186795, it discloses a kind of damping vibration attenuation material, but this material cured condition is 120 DEG C, solidifies 3 hours, does not also relate to Amino Terminated polyether(ATPE) (or polyetheramine) solidifying agent etc.
[summary of the invention]
In order to overcome the deficiency existed in background technology, the invention provides a kind of room temperature curing epoxy base high-damping material and preparation method thereof, main component of the present invention is made up of bisphenol A epoxide resin, polyurethane modified epoxy resin, silane coupling agent, mixing amine curing agent and curing catalyst, the present invention has high damping, and damping temp field width, longer construction working life, can in room temperature environment the feature such as spontaneous curing.
For realizing goal of the invention as above, the present invention adopts technical scheme as described below:
A kind of room temperature curing epoxy base high-damping material, damping material comprises component A and B component, and described component A comprises following composition by weight:
Host 70 ~ 90 parts;
Plasticising-thinner 10 ~ 30 parts;
Silane coupling agent 2 ~ 8 parts;
Described B component comprises following composition by weight:
80 ~ 120 parts, solidifying agent;
Curing catalyst 2 ~ 8 parts;
The proportioning of described component A and B component is 1:(0.8 ~ 1.2).
Described room temperature curing epoxy base high-damping material, described host is bisphenol A epoxide resin and polyurethane modified epoxy resin, and described bisphenol A epoxide resin is the combination of E-44, E-51, CYD-115, CYD-127, CYD-128, CYD-128E, CYD-144 wherein a kind of or any two kinds; Described polyurethane modified epoxy resin is one or both the combination in the polyether(poly)urethane modified epoxy of polyether(poly)urethane modified epoxy and aliphatic glycidyl ether modification.
Described room temperature curing epoxy base high-damping material, the epoxy equivalent (weight) of described polyether(poly)urethane modified epoxy and viscosity are 200 ~ 220g/eg, viscosity (25 DEG C) 50000 ± 7000mpa.s and epoxy equivalent (weight) 250 ~ 270g/eg, viscosity (25 DEG C) 50000 ± 5000mpa.s; The epoxy equivalent (weight) of the polyether(poly)urethane modified epoxy of described aliphatic glycidyl ether modification is 190 ~ 240g/eg, viscosity is (25 DEG C) 13000 ± 3000mpa.s, wherein epoxy resin content is the aliphatic glycidyl ether content of 85 ~ 95%, C12 ~ 14 is 5 ~ 15%.
Described room temperature curing epoxy base high-damping material, described plasticising-thinner comprises any one or two kinds and two or more combinations in ethylene glycol diglycidylether, propylene glycol diglycidylether, neopentylglycol diglycidyl ether and alicyclic cylohexanediol diglycidyl ether.
Described room temperature curing epoxy base high-damping material, described silane coupling agent comprises the combination of any one or two kinds in γ aminopropyltriethoxy silane, γ-(glycidoxy) propyl trimethoxy silicane, γ-mercaptopropyl trimethoxysilane and gamma-mercaptopropyltriethoxysilane.
Described room temperature curing epoxy base high-damping material, described solidifying agent is any one or two or more the combination in aliphatic amide, Amino Terminated polyether(ATPE), polyetheramine and Versamid.
Described room temperature curing epoxy base high-damping material, described aliphatic amide comprises the combination of any one or two kinds in diethylenetriamine, triethylene tetramine, tetraethylene pentamine and polyethylene polyamine; Described Amino Terminated polyether(ATPE) comprises any one or two or more the combination in D-230, D-400, D-2000 and T5000; Described Versamid comprises the combination of any one or two kinds in 200#, 300#, 650#, 651# Versamid.
Described room temperature curing epoxy base high-damping material, described curing catalyst is altax P-30.
A kind of preparation method of room temperature curing epoxy base high-damping material, described preparation method weighs component A and B component first according to a certain percentage respectively, then heat treated is carried out to the host in component A, further, component A and B component are mixed separately respectively in tempering tank, then stir respectively by agitator, grouping barrelling, sealing is preserved.
The preparation method of described room temperature curing epoxy base high-damping material, described host is thermostatically heating 1.5 ~ 2.5h in electric drying oven with forced convection, and heating temperature range is 45 ~ 55 DEG C.
Adopt technical scheme as above, the present invention has following beneficial effect:
A kind of room temperature curing epoxy base high-damping material of the present invention and preparation method thereof, main component of the present invention is by bisphenol A epoxide resin, polyurethane modified epoxy resin, silane coupling agent, mixing amine curing agent and curing catalyst composition, liquid material is divided into A, B two components are prepared burden, by resin first thermostatically heating in electric drying oven with forced convection, stir, and then prepare burden, in tempering tank, each component is mixed separately, stirred by agitator, grouping barrelling, sealing is preserved, namely the preparation of product of the present invention is completed, the present invention has high damping, and damping temp field width, longer construction working life, can in room temperature environment the feature such as spontaneous curing.
[accompanying drawing explanation]
Fig. 1 is the test-results of material loss factor with temperature and change of frequency of the embodiment of the present invention 1;
Fig. 2 is the test-results of material loss factor with temperature and change of frequency of the embodiment of the present invention 2;
Fig. 3 is the test-results of material loss factor with temperature and change of frequency of the embodiment of the present invention 3;
Fig. 4 is the test-results of material loss factor with temperature and change of frequency of the embodiment of the present invention 4.
[embodiment]
Can explain the present invention in more detail by the following examples, the present invention is not limited to the following examples;
A kind of room temperature curing epoxy base high-damping material of the present invention, damping material comprises component A (resin system) and B component (curing system), and described component A comprises following composition by weight:
Host 70 ~ 90 parts; Plasticising-thinner 10 ~ 30 parts;
Silane coupling agent 2 ~ 8 parts;
Described B component comprises following composition by weight:
80 ~ 120 parts, solidifying agent; Curing catalyst 2 ~ 8 parts;
The proportioning of described component A and B component is 1:(0.8 ~ 1.2).
Wherein the composition of resin system is with preferred:
Described host is bisphenol A epoxide resin and polyurethane modified epoxy resin, being the basic ingredient of damping material, is the main body finally forming damping material, and first the mass ratio between three considers damping capacity, next is reaction and rheological property, takes into account the damping characteristic after processing performance and solidification; Wherein said bisphenol A epoxide resin is the combination of E-44, E-51, CYD-115, CYD-127, CYD-128, CYD-128E, CYD-144 wherein a kind of or any two kinds; Described polyurethane modified epoxy resin is one or both the combination in the polyether(poly)urethane modified epoxy of polyether(poly)urethane modified epoxy and aliphatic glycidyl ether modification; The epoxy equivalent (weight) of described polyether(poly)urethane modified epoxy and viscosity are 200 ~ 220g/eg, viscosity (25 DEG C) 50000 ± 7000mpa.s and epoxy equivalent (weight) 250 ~ 270g/eg, viscosity (25 DEG C) 50000 ± 5000mpa.s; The epoxy equivalent (weight) of the polyether(poly)urethane modified epoxy of described aliphatic glycidyl ether modification is 190 ~ 240g/eg, viscosity is (25 DEG C) 13000 ± 3000mpa.s, wherein epoxy resin content is the aliphatic glycidyl ether content of 85 ~ 95%, C12 ~ 14 is 5 ~ 15%; Described plasticising-thinner is a kind of polyol, is glycidyl ether specifically.For reaction speed, the viscosity of system, the second-order transition temperature of cured article, damping temperature domain, Young's modulus etc., comprise any one or two kinds and the two or more combinations in ethylene glycol diglycidylether, propylene glycol diglycidylether, neopentylglycol diglycidyl ether and alicyclic cylohexanediol diglycidyl ether; Described silane coupling agent comprises the combination of any one or two kinds in γ aminopropyltriethoxy silane, γ-(glycidoxy) propyl trimethoxy silicane, γ-mercaptopropyl trimethoxysilane and gamma-mercaptopropyltriethoxysilane.
Wherein the composition of curing system is with preferred:
Described solidifying agent is any one or two or more the combination in aliphatic amide, Amino Terminated polyether(ATPE), polyetheramine and Versamid; Described aliphatic amide comprises the combination of any one or two kinds in diethylenetriamine, triethylene tetramine, tetraethylene pentamine and polyethylene polyamine; Described Amino Terminated polyether(ATPE) comprises any one or two or more the combination in D-230, D-400, D-2000 and T5000; Described Versamid comprises the combination of any one or two kinds in 200#, 300#, 650#, 651# Versamid; Described curing catalyst is altax P-30, is also 2,4,6, three (dimethylamino methyl) phenol.
A kind of preparation method of room temperature curing epoxy base high-damping material, described preparation method weighs component A and B component first according to a certain percentage respectively, then heat treated is carried out to the host in component A, described host is thermostatically heating 1.5 ~ 2.5h in electric drying oven with forced convection, and heating temperature range is 45 ~ 55 DEG C; Further, component A and B component are mixed separately in tempering tank respectively, then stir respectively by agitator, grouping barrelling, sealing is preserved.
The step of the present invention in concrete use procedure is as follows:
One, compound is prepared:
First the component A prepared and B component are carried out mix and blend, after stirring, obtain compound;
Two, bubble is removed to compound:
Connect step, vacuumized under normal temperature condition by the compound that the first step obtains in vaccum-pumping equipment, vacuum gauge pressure is 0.06 ~ 0.1MPa;
Three, cast, embedding:
Connect step, from vaccum-pumping equipment, take out compound, carry out pouring into a mould or embedding, then solidify 20 ~ 28h at ambient temperature, make its primary solidification;
Four, post curing treatment is heated:
Connect step, for material or goods, by the material of primary solidification or goods, put into electric drying oven with forced convection together with mould or frock, wherein the temperature range of electric drying oven with forced convection is 45 ~ 55 DEG C, heating after fixing 68 ~ 76h;
Five, self-vulcanizing:
Connect step, heating after fixing material or goods are taken out together with mould or frock from electric drying oven with forced convection, solidifies 20 ~ 28h at ambient temperature, then the demoulding, or be cut into the size of regulation.
Wherein for impedance bundary, then direct the compound of vacuum defoamation is carried out pouring into a mould or embedding, under natural temperature condition, solidify more than 72h.
Principle of the present invention is: utilize group contribution analytical method, interpenetrating net polymer damping principle, namely urethane and epoxy resin form SPIN (semi-intercrossing network) and IPN (interpenetrating(polymer)networks) structure, these two kinds of structures can play the principle that " forcing mutual tolerance " and " synergistic effect " acts on, the sub-chain motion of polymer molecule and the relation principle of damping, from the system that resin and solidifying agent and adding material are formed, take into account soft, the molecular structure of hard section builds, responded by sub-chain motion when being subject to extraneous vibration or acoustic wave excitation with material, as group sterically hindered, segment composition and distribution, crosslinking structure etc., existing larger sterically hindered, sufficient sub-chain motion response can be carried out again, and the space of suitable sub-chain motion response, the molecular structure factor of such relative quiescent, composition is considered with the combination of the molecule segment exercise factor of relative dynamic, reaction and property relationship, carry out the structure of Material selec-tion and system, by mixing, crosslinked, system material is solidified.Under the target working conditions of setting, high damping properties is possessed so as to realizing system material.
Specific embodiments of the invention are as follows:
Specific embodiments of the invention as following table, during use, first by resin in electric drying oven with forced convection in 50 DEG C of dry 2h, by proportioning weigh, by mixed with resin, stir, add glycidyl ether and silane coupling agent, continue to stir, the component A of constituent material.By aliphatic amide, Amino Terminated polyether(ATPE) and Versamid according to alone or mixed, amplify by proportioning, carry out in advance weighing, prepare burden, be uniformly mixed separately, then again these three kinds of materials are weighed by proportioning, batching, mixing and stirring.Finally add curing catalyst DMP-30 by proportioning, continue to stir, the B component of constituent material.Before using, by the mass ratio of 1:1, accurate weighing A, B component, fully stir, mixing, vacuumizes and remove bubble under room temp, carries out goods cast or for other purposes.Spontaneous curing 24h, is then placed in electric drying oven with forced convection and accelerates solidification 72h in 50 DEG C, then under room temp condition, naturally park solidification 24h.
The dissipation factor tan δ of the embodiment of the present invention 1 ~ 4 is shown in accompanying drawing 1 ~ 4 with the test-results of temperature and change of frequency, and wherein the net effect of embodiment 3 is best.
The formula (weight part) of the specific embodiment of the invention
Compared with prior art, tool has the following advantages in the present invention
From resin and solidifying agent and adding material three directions, take into account soft, the molecular structure of hard section and space steric effect, molecule segment move such relative quiescent with the molecule segment exercise factor of relative dynamic, association reaction and property relationship, segment composition and distribution, crosslinking structure, build Component System, invented material is made to have superior damping capacity, temperature is 10 DEG C, frequency is 10Hz, the highest loss factor t an δ max of material is not less than 1.32, loss Young's modulus is 1.48 × 106Pa, 20Hz material loss factor higher than 0.5 temperature range more than 50 DEG C.By regulating composition and (or) the compound proportion of A, B each component, the damping factor of material or Young's modulus etc. to be regulated very on a large scale.
Material produce of the present invention and construction technology are simple, easy to operate, are suitable for suitability for industrialized production and through engineering approaches is applied.
Part not in the detailed description of the invention is prior art.
The embodiment selected in this article in order to open object of the present invention, currently thinks to be suitable for, but it is to be understood that the present invention is intended to comprise all changes belonging to the embodiment in this design and invention scope and improvement.
Claims (10)
1. a room temperature curing epoxy base high-damping material, is characterized in that: damping material comprises component A and B component, and described component A comprises following composition by weight:
Host 70 ~ 90 parts;
Plasticising-thinner 10 ~ 30 parts;
Silane coupling agent 2 ~ 8 parts;
Described B component comprises following composition by weight:
80 ~ 120 parts, solidifying agent;
Curing catalyst 2 ~ 8 parts;
The proportioning of described component A and B component is 1:(0.8 ~ 1.2).
2. room temperature curing epoxy base high-damping material according to claim 1, it is characterized in that: described host is bisphenol A epoxide resin and polyurethane modified epoxy resin, described bisphenol A epoxide resin is the combination of E-44, E-51, CYD-115, CYD-127, CYD-128, CYD-128E, CYD-144 wherein a kind of or any two kinds; Described polyurethane modified epoxy resin is one or both the combination in the polyether(poly)urethane modified epoxy of polyether(poly)urethane modified epoxy and aliphatic glycidyl ether modification.
3. room temperature curing epoxy base high-damping material according to claim 2, it is characterized in that: the epoxy equivalent (weight) of described polyether(poly)urethane modified epoxy and viscosity are 200 ~ 220g/eg, viscosity (25 DEG C) 50000 ± 7000mpa.s and epoxy equivalent (weight) 250 ~ 270g/eg, viscosity (25 DEG C) 50000 ± 5000mpa.s; The epoxy equivalent (weight) of the polyether(poly)urethane modified epoxy of described aliphatic glycidyl ether modification is 190 ~ 240g/eg, viscosity is (25 DEG C) 13000 ± 3000mpa.s, wherein epoxy resin content is the aliphatic glycidyl ether content of 85 ~ 95%, C12 ~ 14 is 5 ~ 15%.
4. room temperature curing epoxy base high-damping material according to claim 1, is characterized in that: described plasticising-thinner comprises any one or two kinds and two or more combinations in ethylene glycol diglycidylether, propylene glycol diglycidylether, neopentylglycol diglycidyl ether and alicyclic cylohexanediol diglycidyl ether.
5. room temperature curing epoxy base high-damping material according to claim 1, is characterized in that: described silane coupling agent comprises the combination of any one or two kinds in γ aminopropyltriethoxy silane, γ-(glycidoxy) propyl trimethoxy silicane, γ-mercaptopropyl trimethoxysilane and gamma-mercaptopropyltriethoxysilane.
6. room temperature curing epoxy base high-damping material according to claim 1, is characterized in that: described solidifying agent is any one or two or more the combination in aliphatic amide, Amino Terminated polyether(ATPE), polyetheramine and Versamid.
7. room temperature curing epoxy base high-damping material according to claim 1, is characterized in that: described aliphatic amide comprises the combination of any one or two kinds in diethylenetriamine, triethylene tetramine, tetraethylene pentamine and polyethylene polyamine; Described Amino Terminated polyether(ATPE) comprises any one or two or more the combination in D-230, D-400, D-2000 and T5000; Described Versamid comprises the combination of any one or two kinds in 200#, 300#, 650#, 651# Versamid.
8. room temperature curing epoxy base high-damping material according to claim 1, is characterized in that: described curing catalyst is altax P-30.
9. implement the claims the preparation method of a kind of room temperature curing epoxy base high-damping material of a kind of room temperature curing epoxy base high-damping material described in 1 ~ 8 arbitrary claim, it is characterized in that: described preparation method weighs component A and B component first according to a certain percentage respectively, then heat treated is carried out to the host in component A, further, component A and B component are mixed separately respectively in tempering tank, then stir respectively by agitator, grouping barrelling, sealing is preserved.
10. the preparation method of room temperature curing epoxy base high-damping material according to claim 9, it is characterized in that: the preparation method of described room temperature curing epoxy base high-damping material, described host is thermostatically heating 1.5 ~ 2.5h in electric drying oven with forced convection, and heating temperature range is 45 ~ 55 DEG C.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106633640A (en) * | 2016-11-28 | 2017-05-10 | 青岛海尔特种电冰柜有限公司 | Damping composite material, damping pressing machine bottom plate structure and refrigerator |
| CN107815070A (en) * | 2017-11-09 | 2018-03-20 | 湖北航天化学技术研究所 | A kind of room temperature-curing low-viscosity high strength epoxy resin castable and preparation method |
| CN113754345A (en) * | 2021-09-22 | 2021-12-07 | 山东硕果新材料科技有限公司 | High-damping resin-based mineral composite material and preparation method and application thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5331062A (en) * | 1991-08-28 | 1994-07-19 | The United States Of America As Represented By The Secretary Of The Navy | Polyurethane-epoxy interpenetrating polymer network acoustic damping material |
| CN103320073A (en) * | 2013-06-26 | 2013-09-25 | 株洲世林聚合物有限公司 | Pouring type epoxy resin-based high-damping encapsulation material |
| CN103965589A (en) * | 2014-05-14 | 2014-08-06 | 武汉理工大学 | Piezoelectric damping polymer vibration isolation gasket and preparation method thereof |
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2015
- 2015-04-30 CN CN201510216412.3A patent/CN104845045A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5331062A (en) * | 1991-08-28 | 1994-07-19 | The United States Of America As Represented By The Secretary Of The Navy | Polyurethane-epoxy interpenetrating polymer network acoustic damping material |
| CN103320073A (en) * | 2013-06-26 | 2013-09-25 | 株洲世林聚合物有限公司 | Pouring type epoxy resin-based high-damping encapsulation material |
| CN103965589A (en) * | 2014-05-14 | 2014-08-06 | 武汉理工大学 | Piezoelectric damping polymer vibration isolation gasket and preparation method thereof |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106633640A (en) * | 2016-11-28 | 2017-05-10 | 青岛海尔特种电冰柜有限公司 | Damping composite material, damping pressing machine bottom plate structure and refrigerator |
| CN106633640B (en) * | 2016-11-28 | 2019-05-31 | 青岛海尔特种电冰柜有限公司 | Damp composite material, damping compression plate structure and ice box |
| CN107815070A (en) * | 2017-11-09 | 2018-03-20 | 湖北航天化学技术研究所 | A kind of room temperature-curing low-viscosity high strength epoxy resin castable and preparation method |
| CN113754345A (en) * | 2021-09-22 | 2021-12-07 | 山东硕果新材料科技有限公司 | High-damping resin-based mineral composite material and preparation method and application thereof |
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