CN105733484A - Toughening-modified epoxy resin adhesive and preparation method thereof - Google Patents
Toughening-modified epoxy resin adhesive and preparation method thereof Download PDFInfo
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- CN105733484A CN105733484A CN201610186366.1A CN201610186366A CN105733484A CN 105733484 A CN105733484 A CN 105733484A CN 201610186366 A CN201610186366 A CN 201610186366A CN 105733484 A CN105733484 A CN 105733484A
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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
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F283/00—Macromolecular compounds obtained by polymerising monomers on to polymers provided for in subclass C08G
- C08F283/006—Macromolecular compounds obtained by polymerising monomers on to polymers provided for in subclass C08G on to polymers provided for in C08G18/00
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F283/00—Macromolecular compounds obtained by polymerising monomers on to polymers provided for in subclass C08G
- C08F283/04—Macromolecular compounds obtained by polymerising monomers on to polymers provided for in subclass C08G on to polycarbonamides, polyesteramides or polyimides
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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
-
- 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
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/011—Nanostructured additives
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/02—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group
- C08L2205/025—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group containing two or more polymers of the same hierarchy C08L, and differing only in parameters such as density, comonomer content, molecular weight, structure
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- 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
Abstract
The invention discloses a toughening-modified epoxy resin adhesive and a preparation method thereof. The toughening-modified epoxy resin adhesive comprises 25-55 parts of epoxy resin, 12-28 parts of polyurethane, 8-19 parts of polyimide, 6-18 parts of nano silicon carbide, 7-21 parts of polyethersulfone, 5-14 parts of silicon dioxide, 7-15 parts of acrylate, 2-11 parts of titanium dioxide, 2-8 parts of meta-hydroxy biphenyl, 3-9 parts of meta-trifluoromethyl phenol, 13-24 parts of isopropylketone, 12-26 parts of sodium carbonate and 24-42 parts of water. By using the polyurethane and epoxy resin for modification, the prepared epoxy resin adhesive has the advantages of high toughness and high strength.
Description
Technical field
The present invention relates to adhesive field, particularly relate to a kind of Toughening Modification of Epoxy adhesive and preparation method thereof.
Background technology
Epoxy resin (EP) adhesive is that a kind of adhesive property is good, applies very general adhesive.Epoxy resin has many advantages, such as excellent chemical stability, corrosion resistance, electrical apparatus insulation and shrinkage factor are low, easy machine-shaping etc..High yet with crosslink density after single epoxy resin cure, in tridimensional network, there is internal stress big, matter is crisp, poor impact resistance, it is easy to the shortcomings such as cracking, it is difficult to meet engineering requirement so that it is application is subject to certain restrictions.For a long time, epoxy resin is carried out toughening modifying and be always up an important research contents.Polyurethane (PU) is the macromolecular material of a class function admirable, there is high impact strength and excellent resistance to low temperature, both can be made to have complementary advantages with polyurethane modified epoxy resin adhesive, obtain a kind of not only there is certain pliability but also there is the more satisfactory adhesive of fine adhesion strength.
The research of polyurethane modified epoxy resin starts from the sixties in 20th century, and first DowChemical company of the U.S. succeeds in developing.Polyurethane modified epoxy resin structural adhesive, can be used for Aero-Space industry.In recent decades, epoxy resin roughening technology has been carried out substantial amounts of research by domestic and international researcher, polyurethane toughened modified epoxy technology has had and has developed on a large scale very much, wherein forms interpenetrating net polymer Toughening Modification of Epoxy with polyurethane and epoxy resin the most noticeable.
But, although directly adopting the adhesive toughening effect that epoxy resin modification is prepared by polyurethane to be improved in prior art, but its solidification temperature is high, and the heat distortion temperature of cured product is low；In addition, being mostly of studies in China is blended, IPN or semi-intercrossing network modifier, only have minority unit and develop solvent-free products, and foreign study be mostly solvent based product, domestic method for toughening is nearly all to sacrifice modified mechanics performance for cost, it is difficult to make the toughness of epoxy resin and intensity improve simultaneously.
Summary of the invention
Present invention solves the technical problem that and be: the epoxy resin adhesive improved to obtain a kind of toughness and intensity to obtain simultaneously, the invention provides a kind of Toughening Modification of Epoxy adhesive and preparation method thereof.
Technical scheme: a kind of Toughening Modification of Epoxy adhesive, comprises following components: epoxy resin 25～55 parts, polyurethane 12～28 parts, polyimides 8～19 parts, nanometer silicon carbide 6～18 parts, polyether sulfone 7～21 parts, silicon dioxide 5～14 parts, acrylate 7～15 parts, titanium dioxide 2～11 part, xenol 2～8 parts, m-trifluoromethyl phenol 3～9 parts, isopropyl acetone 13～24 parts, sodium carbonate 12～26 parts, 24～42 parts of water.
Preferably, described Toughening Modification of Epoxy adhesive comprises following components: epoxy resin 48 parts, polyurethane 23 parts, polyimides 14 parts, nanometer silicon carbide 15 parts, polyether sulfone 17 parts, silica 11 part, acrylate 12 parts, titanium dioxide 7 part, xenol 5 parts, m-trifluoromethyl phenol 6 parts, isopropyl acetone 19 parts, sodium carbonate 21 parts, 36 parts of water.
The preparation method of a kind of Toughening Modification of Epoxy adhesive, comprises the steps of
(1) prepared by modified polyurethane: polyurethane, polyimides, nanometer silicon carbide, silicon dioxide and acrylate are added in reactor, and reaction temperature is 560～780 DEG C, pressure is 1.8～3.8MPa, blender rotating speed is 1200～2400 revs/min, the response time is 18～40 minutes；
(2) prepared by modified epoxy: sodium carbonate is soluble in water, epoxy resin, polyether sulfone, titanium dioxide, an xenol and m-trifluoromethyl phenol are added in aqueous sodium carbonate, after mix homogeneously, reacting by heating, reaction terminates rear evaporation of solvent, adds isopropyl acetone, is washed with water and washs, remove aqueous phase, organic facies is evaporated to and does and obtain modified epoxy；
(3) prepared by adhesive: modified polyurethane step (1) prepared adds in the modified epoxy that step (2) obtains, it is placed in the oil bath pan of 110～130 DEG C, open mulser, with the speed continuous shear stress 25～45 minutes of 2000～6000 revs/min, add stabilizer 2～18 parts and mulser rotating speed is adjusted to 600～1200 revs/min, after stirring 15～30 minutes, can be prepared by Toughening Modification of Epoxy adhesive.
Preferably, polyurethane, polyimides, nanometer silicon carbide, silicon dioxide and acrylate being added in reactor in step (1), reaction temperature is 690 DEG C, pressure is 3.2MPa, blender rotating speed is 2000 revs/min, the response time is 32 minutes.
Preferably, modified polyurethane step (1) prepared in step (3) adds in the modified epoxy that step (2) obtains, it is placed in the oil bath pan of 122 DEG C, open mulser, with the speed continuous shear stress 38 minutes of 4000 revs/min, add stabilizer 11 parts and mulser rotating speed is adjusted to 1000 revs/min, after stirring 23 minutes, can be prepared by Toughening Modification of Epoxy adhesive.
Beneficial effect: the present invention is by being modified polyurethane and epoxy resin, and the epoxy resin adhesive prepared has the advantage that toughness is strong, intensity is high.
Detailed description of the invention
Embodiment 1
A kind of Toughening Modification of Epoxy adhesive, comprises following components: epoxy resin 25 parts, polyurethane 12 parts, polyimides 8 parts, nanometer silicon carbide 6 parts, polyether sulfone 7 parts, silicon dioxide 5 parts, acrylate 7 parts, titanium dioxide 2 part, xenol 2 parts, m-trifluoromethyl phenol 3 parts, isopropyl acetone 13 parts, sodium carbonate 12 parts, 24 parts of water.
The preparation method of a kind of Toughening Modification of Epoxy adhesive, comprises the steps of
(1) prepared by modified polyurethane: polyurethane, polyimides, nanometer silicon carbide, silicon dioxide and acrylate are added in reactor, and reaction temperature is 560 DEG C, pressure is 1.8MPa, blender rotating speed is 1200 revs/min, the response time is 18 minutes；
(2) prepared by modified epoxy: sodium carbonate is soluble in water, epoxy resin, polyether sulfone, titanium dioxide, an xenol and m-trifluoromethyl phenol are added in aqueous sodium carbonate, after mix homogeneously, reacting by heating, reaction terminates rear evaporation of solvent, adds isopropyl acetone, is washed with water and washs, remove aqueous phase, organic facies is evaporated to and does and obtain modified epoxy；
(3) prepared by adhesive: modified polyurethane step (1) prepared adds in the modified epoxy that step (2) obtains, it is placed in the oil bath pan of 110 DEG C, open mulser, with the speed continuous shear stress 25 minutes of 2000 revs/min, add stabilizer 2 parts and mulser rotating speed is adjusted to 600 revs/min, after stirring 15 minutes, can be prepared by Toughening Modification of Epoxy adhesive.
Embodiment 2
A kind of Toughening Modification of Epoxy adhesive, comprises following components: epoxy resin 48 parts, polyurethane 23 parts, polyimides 14 parts, nanometer silicon carbide 15 parts, polyether sulfone 17 parts, silica 11 part, acrylate 12 parts, titanium dioxide 7 part, xenol 5 parts, m-trifluoromethyl phenol 6 parts, isopropyl acetone 19 parts, sodium carbonate 21 parts, 36 parts of water.
The preparation method of a kind of Toughening Modification of Epoxy adhesive, comprises the steps of
(1) prepared by modified polyurethane: polyurethane, polyimides, nanometer silicon carbide, silicon dioxide and acrylate are added in reactor, and reaction temperature is 690 DEG C, pressure is 3.2MPa, blender rotating speed is 2000 revs/min, the response time is 32 minutes；
(2) prepared by modified epoxy: sodium carbonate is soluble in water, epoxy resin, polyether sulfone, titanium dioxide, an xenol and m-trifluoromethyl phenol are added in aqueous sodium carbonate, after mix homogeneously, reacting by heating, reaction terminates rear evaporation of solvent, adds isopropyl acetone, is washed with water and washs, remove aqueous phase, organic facies is evaporated to and does and obtain modified epoxy；
(3) prepared by adhesive: modified polyurethane step (1) prepared adds in the modified epoxy that step (2) obtains, it is placed in the oil bath pan of 122 DEG C, open mulser, with the speed continuous shear stress 38 minutes of 4000 revs/min, add stabilizer 11 parts and mulser rotating speed is adjusted to 1000 revs/min, after stirring 23 minutes, can be prepared by Toughening Modification of Epoxy adhesive.
Embodiment 3
A kind of Toughening Modification of Epoxy adhesive, comprises following components: epoxy resin 55 parts, polyurethane 28 parts, polyimides 19 parts, nanometer silicon carbide 18 parts, polyether sulfone 21 parts, silica 14 parts, acrylate 15 parts, titanium dioxide 11 part, xenol 8 parts, m-trifluoromethyl phenol 9 parts, isopropyl acetone 24 parts, sodium carbonate 26 parts, 42 parts of water.
The preparation method of a kind of Toughening Modification of Epoxy adhesive, comprises the steps of
(1) prepared by modified polyurethane: polyurethane, polyimides, nanometer silicon carbide, silicon dioxide and acrylate are added in reactor, and reaction temperature is 780 DEG C, pressure is 3.8MPa, blender rotating speed is 2400 revs/min, the response time is 40 minutes；
(2) prepared by modified epoxy: sodium carbonate is soluble in water, epoxy resin, polyether sulfone, titanium dioxide, an xenol and m-trifluoromethyl phenol are added in aqueous sodium carbonate, after mix homogeneously, reacting by heating, reaction terminates rear evaporation of solvent, adds isopropyl acetone, is washed with water and washs, remove aqueous phase, organic facies is evaporated to and does and obtain modified epoxy；
(3) prepared by adhesive: modified polyurethane step (1) prepared adds in the modified epoxy that step (2) obtains, it is placed in the oil bath pan of 130 DEG C, open mulser, with the speed continuous shear stress 45 minutes of 6000 revs/min, add stabilizer 18 parts and mulser rotating speed is adjusted to 1200 revs/min, after stirring 30 minutes, can be prepared by Toughening Modification of Epoxy adhesive.
The Toughening Modification of Epoxy adhesive that above-described embodiment 1～3 is prepared carries out performance detection, and result is as shown in table 1:
The Toughening Modification of Epoxy adhesive that table 1 embodiment 1～3 prepares carries out performance test results
Claims (5)
1. a Toughening Modification of Epoxy adhesive, it is characterized in that, comprise following components: epoxy resin 25～55 parts, polyurethane 12～28 parts, polyimides 8～19 parts, nanometer silicon carbide 6～18 parts, polyether sulfone 7～21 parts, silicon dioxide 5～14 parts, acrylate 7～15 parts, titanium dioxide 2～11 part, xenol 2～8 parts, m-trifluoromethyl phenol 3～9 parts, isopropyl acetone 13～24 parts, sodium carbonate 12～26 parts, 24～42 parts of water.
2. a kind of Toughening Modification of Epoxy adhesive according to claim 1, it is characterized in that, comprise following components: epoxy resin 48 parts, polyurethane 23 parts, polyimides 14 parts, nanometer silicon carbide 15 parts, polyether sulfone 17 parts, silica 11 part, acrylate 12 parts, titanium dioxide 7 part, xenol 5 parts, m-trifluoromethyl phenol 6 parts, isopropyl acetone 19 parts, sodium carbonate 21 parts, 36 parts of water.
3. the preparation method of a kind of Toughening Modification of Epoxy adhesive described in claim 1, it is characterised in that comprise the steps of
(1) prepared by modified polyurethane: polyurethane, polyimides, nanometer silicon carbide, silicon dioxide and acrylate are added in reactor, and reaction temperature is 560～780 DEG C, pressure is 1.8～3.8MPa, blender rotating speed is 1200～2400 revs/min, the response time is 18～40 minutes；
(2) prepared by modified epoxy: sodium carbonate is soluble in water, epoxy resin, polyether sulfone, titanium dioxide, an xenol and m-trifluoromethyl phenol are added in aqueous sodium carbonate, after mix homogeneously, reacting by heating, reaction terminates rear evaporation of solvent, adds isopropyl acetone, is washed with water and washs, remove aqueous phase, organic facies is evaporated to and does and obtain modified epoxy；
(3) prepared by adhesive: modified polyurethane step (1) prepared adds in the modified epoxy that step (2) obtains, it is placed in the oil bath pan of 110～130 DEG C, open mulser, with the speed continuous shear stress 25～45 minutes of 2000～6000 revs/min, add stabilizer 2～18 parts and mulser rotating speed is adjusted to 600～1200 revs/min, after stirring 15～30 minutes, can be prepared by Toughening Modification of Epoxy adhesive.
4. the preparation method of a kind of Toughening Modification of Epoxy adhesive according to claim 3, it is characterized in that, polyurethane, polyimides, nanometer silicon carbide, silicon dioxide and acrylate being added in reactor in step (1), reaction temperature is 690 DEG C, pressure is 3.2MPa, blender rotating speed is 2000 revs/min, the response time is 32 minutes.
5. the preparation method of a kind of Toughening Modification of Epoxy adhesive according to claim 3, it is characterized in that, modified polyurethane step (1) prepared in step (3) adds in the modified epoxy that step (2) obtains, it is placed in the oil bath pan of 122 DEG C, open mulser, with the speed continuous shear stress 38 minutes of 4000 revs/min, add stabilizer 11 parts and mulser rotating speed is adjusted to 1000 revs/min, after stirring 23 minutes, can be prepared by Toughening Modification of Epoxy adhesive.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201610186366.1A CN105733484A (en) | 2016-03-29 | 2016-03-29 | Toughening-modified epoxy resin adhesive and preparation method thereof |
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| CN201610186366.1A CN105733484A (en) | 2016-03-29 | 2016-03-29 | Toughening-modified epoxy resin adhesive and preparation method thereof |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110815683A (en) * | 2019-10-18 | 2020-02-21 | 温州大学 | PTFE composite grid plate |
| CN113795561A (en) * | 2019-05-06 | 2021-12-14 | 中路交科科技股份有限公司 | Fatigue-resistant cold-mixed epoxy resin material, preparation method and application thereof |
| CN114256563A (en) * | 2021-12-20 | 2022-03-29 | 东莞新能源科技有限公司 | Conductive adhesive, electrochemical device, and electronic device |
| CN114836161A (en) * | 2022-05-30 | 2022-08-02 | 郑春华 | Preparation process of blending modified polyurethane adhesive |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101675137A (en) * | 2007-04-30 | 2010-03-17 | Lg化学株式会社 | Adhesive resin composition and dicing die bonding film using the same |
| CN104789175A (en) * | 2015-03-06 | 2015-07-22 | 国家纳米科学中心 | Insulating and thermal conductive ablation resistant adhesive and application thereof in lightning protection |
-
2016
- 2016-03-29 CN CN201610186366.1A patent/CN105733484A/en not_active Withdrawn
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101675137A (en) * | 2007-04-30 | 2010-03-17 | Lg化学株式会社 | Adhesive resin composition and dicing die bonding film using the same |
| CN104745131A (en) * | 2007-04-30 | 2015-07-01 | Lg化学株式会社 | Adhesive Resin Composition And Dicing Die Bonding Film Using The Same |
| CN104789175A (en) * | 2015-03-06 | 2015-07-22 | 国家纳米科学中心 | Insulating and thermal conductive ablation resistant adhesive and application thereof in lightning protection |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113795561A (en) * | 2019-05-06 | 2021-12-14 | 中路交科科技股份有限公司 | Fatigue-resistant cold-mixed epoxy resin material, preparation method and application thereof |
| CN110815683A (en) * | 2019-10-18 | 2020-02-21 | 温州大学 | PTFE composite grid plate |
| CN114256563A (en) * | 2021-12-20 | 2022-03-29 | 东莞新能源科技有限公司 | Conductive adhesive, electrochemical device, and electronic device |
| CN114836161A (en) * | 2022-05-30 | 2022-08-02 | 郑春华 | Preparation process of blending modified polyurethane adhesive |
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