CN108570217A - A kind of preparation method and applications of high transparency epoxy resin composite material - Google Patents
A kind of preparation method and applications of high transparency epoxy resin composite material Download PDFInfo
- Publication number
- CN108570217A CN108570217A CN201810458991.6A CN201810458991A CN108570217A CN 108570217 A CN108570217 A CN 108570217A CN 201810458991 A CN201810458991 A CN 201810458991A CN 108570217 A CN108570217 A CN 108570217A
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- epoxy resin
- composite material
- temperature
- high transparency
- preparation
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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
- C08L63/00—Compositions of epoxy resins; Compositions of derivatives of epoxy resins
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/08—Stabilised against heat, light or radiation or oxydation
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/10—Transparent films; Clear coatings; Transparent materials
-
- 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 kind of preparation methods of high transparency epoxy resin composite material, include the following steps:(1) by liquid-state epoxy resin and solid epoxy resin be 110 140 DEG C in temperature at mix, obtain mixed liquor A;(2) by above-mentioned mixed liquor A and ultraviolet-resistant aid be 110 120 DEG C in temperature at mix, obtain mixed liquid B;(3) curing agent is added into above-mentioned mixed liquid B, is mixed at being 60 70 DEG C in temperature, obtains mixed liquor C;(4) accelerating agent is added into above-mentioned mixed liquor C, after being stirred at being 60 70 DEG C in temperature, casts on stainless steel mould, the high-transparence composite is obtained after solidification demoulding.The composite material of the present invention has color inhibition characteristic under higher high temperature, has huge application prospect in the more demanding field of material transparent.
Description
Technical field
The invention belongs to field of polymer material preparing technology, and in particular to a kind of high transparency epoxy resin composite material
Preparation method and applications.
Background technology
With the rapid development of economic construction of China, the requirement to various circuit devcies, motor is continuously improved, and circuit device
Part, motor easy to produce a large amount of heat during the work time, and seriously affect electric appliance, reliability, the stability that motor works
With service life etc..Therefore, it is necessary to develop new high transparency, the encapsulating material of stability.Epoxy resin is used in encapsulating material
Measure one of maximum plastic products.
But color is easy to turn yellow epoxy resin under the high temperature conditions, has seriously affected the appearance of carbon fiber product, has applied
People has been devoted to solve the problems, such as this, and such as application No. is utilized in epoxy-resin systems in 201510412892.0 patent
Color inhibition auxiliary agent is added so that the epoxy resin composite material toasts 2 hours in 170 DEG C of baking ovens, and composite material is existing without turning yellow
As bending strength reaches 130Mpa, tensile strength 80Mpa, mist degree 2.1%, 45 ° of glossiness 120.8%.But
Invention content
Goal of the invention:The purpose of the present invention is to provide a kind of preparation method of high transparency epoxy resin composite material and its
Using the composite material has color inhibition characteristic under higher high temperature, has in the more demanding field of material transparent huge
Application prospect.
Technical solution:A kind of preparation method of high transparency epoxy resin composite material of the present invention, including following step
Suddenly:(1) liquid-state epoxy resin and solid epoxy resin are stirred into 20-30min in the case where temperature is 110-140 DEG C, mixing is complete
Afterwards, mixed liquor A is obtained;The mass ratio of the solid epoxy resin and liquid-state epoxy resin is 5:1-5;(2) by above-mentioned mixed liquor A
With ultraviolet-resistant aid in the case where temperature is 110-120 DEG C, stirs 15-30min and obtain mixed liquid B after mixing completely;The mixing
The mass ratio of liquid A and ultraviolet-resistant aid is 100:0.2-0.5;(3) curing agent is added into above-mentioned mixed liquid B, is 60- in temperature
At 70 DEG C, 10-20min is stirred, after stirring evenly, obtains mixed liquor C;The mass ratio of the mixed liquid B and curing agent is 100:
2-2.5;(4) accelerating agent is added into above-mentioned mixed liquor C, in the case where temperature is 60-70 DEG C, after stirring 10-20min is stirred evenly,
It casts on stainless steel mould, the high-transparence composite is obtained after solidification demoulding;The mass ratio of the mixed liquor C and accelerating agent
It is 100:0.5-5.
In step (1), the liquid-state epoxy resin is one or more in bisphenol A-type 128, E44 and E51.It is described
Solid epoxy resin is one or more in 901,904,907 and E20 of bisphenol A-type.
Further, the liquid-state epoxy resin is 3 by mass ratio:1 bisphenol A-type 128 is formed with E51;The solid-state
Epoxy resin is 1 by mass ratio:2 bisphenol A-type 901 and 907 forms.
In step (2), the ultraviolet-resistant aid is one or more in UV968 and UV967.
Further, the ultraviolet-resistant aid is 3 by mass ratio:5 UV968 and UV967 composition.
In step (3), the curing agent is one or more in dicyandiamide 100S, 100SF, acid anhydrides and DDA-5.
In step (4), the accelerating agent is one or more in two ureas U-24M, UR300 and UR500.
Further, mixed liquor A described in step (2) and the whipping temp of ultraviolet-resistant aid agent are than described in step (3)
The whipping temp of mixed liquid B and curing agent is 50 DEG C high.
The whipping temp of mixed liquid B and curing agent described in step (3) than in mixed liquor C described in step (4) with promotion
The whipping temp of agent is identical.
Advantageous effect:(1) present invention has the characteristics such as good color inhibition using ultraviolet-resistant aid, by ultraviolet-resistant aid point
It is dispersed in epoxy-resin systems, in combination with the mechanical property that epoxy resin is excellent, makes composite material table in use
Reveal good yellowing resistance characteristic;(2) optimize composite material preparation temperature so that composite system is more uniform, has
Good mechanical property;(3) high transparency epoxy resin composite material preparation method of the invention is simple, efficient, at low cost, work
The production of industry metaplasia has a high potential, and products obtained therefrom has the characteristics such as high color inhibition and high intensity.
Specific implementation mode
In order to better understand the present invention, described herein with reference to the embodiment content that the present invention is furture elucidated
Specific examples are only used to explain the present invention, is not intended to limit the present invention.
Embodiment 1:67 grams of solid epoxy resin bisphenol A-types 901 and 33 grams of liquid-state epoxy resin bisphenol A-types 128 are placed in
In 500 milliliters of the glass flask with vacuum plant, at 110 DEG C, 30min is stirred, solution A is obtained, be directly used in next step
Reaction;
Solution A and 0.2 gram of ultraviolet-resistant aid UV968 are placed in 500 milliliters of the glass flask with vacuum plant,
Temperature is to stir 20min at 110 DEG C, obtains solution B;
2 grams of curing agent dicyandiamide 100S will be added in solution B, 20min is stirred at 60 DEG C, obtains mixed liquor C;
0.8 gram of accelerating agent UR500 will be added in upper step mixed liquor C, in the case where temperature is 60 DEG C, stirs 10min, mixed
Object D;
Mixed liquor D is cast on stainless steel mould, 160 DEG C of one hours of solidification, the high transparency epoxy is obtained after demoulding
Resin composite materials.
Embodiment 2:67 grams of solid epoxy bisphenol A-types 904 and 33 grams of liquid-state epoxy resin bisphenol A-type E44 are placed in
In 500 milliliters of the glass flask with vacuum plant, under the conditions of temperature is 140 DEG C, 20min is stirred, mixed liquor A is obtained,
It is directly used in and reacts in next step;
Mixed liquor A and 0.5 gram of ultraviolet-resistant aid UV967 are placed in 500 milliliters of the glass flask with vacuum plant,
30min is stirred at being 120 DEG C in temperature, obtains mixed liquid B;
2 grams of curing agent dicyandiamide 100SF will be added in mixed liquid B, 10min is stirred at 70 DEG C, obtains mixed liquor C;
3 grams of accelerating agent UR500 will be added in upper step mixed liquor C, in the case where temperature is 70 DEG C, stirs 20min, obtain mixed liquor
D;
Mixed liquor D is cast on stainless steel mould, 160 DEG C of one hours of solidification, the high transparency epoxy is obtained after demoulding
Resin composite materials.
Embodiment 3:By 22 grams of bisphenol A-types 901 of solid epoxy and 45 grams of bisphenol A-types 907 and liquid epoxies 25
Gram bisphenol A-type 128 and 8 grams of bisphenol A-type E51 are placed in 500 milliliters of the glass flask with vacuum plant, at 120 DEG C, stirring
30min obtains mixed liquor A, is directly used in and reacts in next step;
Mixed liquor A and 0.15 gram of ultraviolet-resistant aid UV968 and 0.25 gram of ultraviolet-resistant aid UV967 are placed in 500 milliliters
In glass flask with vacuum plant, 20min is stirred at being 110 DEG C in temperature, obtains mixed liquid B;
2 grams of curing agent dicyandiamide DDA-5 will be added in mixed liquid B, 20min is stirred at 60 DEG C, obtains mixed liquor C;
3 grams of accelerating agent UR300 will be added in upper step mixed liquor C, in the case where temperature is 60 DEG C, stirs 10min, obtain mixture
D;
Mixed liquor D is cast on stainless steel mould, 160 DEG C of one hours of solidification, the high transparency epoxy is obtained after demoulding
Resin composite materials.
Comparative example 1:Without ultraviolet-resistant aid, remaining is the same as embodiment 3.
Comparative example 2:By 22 grams of bisphenol A-types 901 of solid epoxy and 45 grams of bisphenol A-types 907 and liquid epoxies 25
Gram bisphenol A-type 128 and 8 grams of bisphenol A-type E51 are placed in 500 milliliters of the glass flask with vacuum plant, at 120 DEG C, stirring
30min obtains mixed liquor A, is directly used in and reacts in next step;
Mixed liquor A and 0.15 gram of ultraviolet-resistant aid UV968 and 0.25 gram of ultraviolet-resistant aid UV967 are placed in 500 milliliters
In glass flask with vacuum plant, 20min is stirred at being 110 DEG C in temperature, obtains mixed liquid B;
2 grams of curing agent dicyandiamide DDA-5 will be added in mixed liquid B, 20min is stirred at 70 DEG C, obtains mixed liquor C;
3 grams of accelerating agent UR300 will be added in upper step mixed liquor C, in the case where temperature is 60 DEG C, stirs 10min, obtain mixture
D;
Mixed liquor D is cast on stainless steel mould, 160 DEG C of one hours of solidification, the high transparency epoxy is obtained after demoulding
Resin composite materials.
Two, sample detection methods
Toasted 2 hours in 170 DEG C of baking ovens in the high transparency epoxy resin composite material of preparation, measure composite material without
Yellowing.
Three, testing result
The testing result of 1 properties of sample of table
It can be seen from the result of table 1 when ultraviolet-resistant aid is added in the composite, the anti-yellowing of material can be increased
Become performance, in addition, adjustment material composition ratio so that composite material have better mechanics effect, and it is a discovery of the invention that
At a temperature of specific blend, the uniform performance and comprehensive performance of material are better.
Claims (10)
1. a kind of preparation method of high transparency epoxy resin composite material, which is characterized in that include the following steps:
(1) liquid-state epoxy resin and solid epoxy resin are stirred into 20-30min in the case where temperature is 110-140 DEG C, mixing is complete
Afterwards, mixed liquor A is obtained;The mass ratio of the solid epoxy resin and liquid-state epoxy resin is 5:1-5;
(2) above-mentioned mixed liquor A and ultraviolet-resistant aid are stirred into 15-30min in the case where temperature is 110-120 DEG C, after mixing completely,
Obtain mixed liquid B;The mass ratio of the mixed liquor A and ultraviolet-resistant aid is 100:0.2-0.5;
(3) curing agent is added into above-mentioned mixed liquid B, in the case where temperature is 60-70 DEG C, stirs 10-20min, after stirring evenly, obtain
To mixed liquor C;The mass ratio of the mixed liquid B and curing agent is 100:2-2.5;
(4) accelerating agent is added into above-mentioned mixed liquor C, in the case where temperature is 60-70 DEG C, stirs 10-20min, after stirring evenly, pour
Casting obtains the high-transparence composite on stainless steel mould after solidification demoulding;The mass ratio of the mixed liquor C and accelerating agent is
100:0.5-5。
2. the preparation method of high transparency epoxy resin composite material according to claim 1, it is characterised in that step (1)
In, the liquid-state epoxy resin is one or more in bisphenol A-type 128, E44 and E51.
3. the preparation method of high transparency epoxy resin composite material according to claim 1, it is characterised in that step (1)
In, the solid epoxy resin is one or more in 901,904,907 and E20 of bisphenol A-type.
4. the preparation method of high transparency epoxy resin composite material according to claim 1, it is characterised in that step (2)
In, the ultraviolet-resistant aid is one or more in UV968 and UV967.
5. the preparation method of high transparency epoxy resin composite material according to claim 1, it is characterised in that step (3)
In, the curing agent is one or more in dicyandiamide 100S, 100SF, acid anhydrides and DDA-5.
6. the preparation method of high transparency epoxy resin composite material according to claim 1, it is characterised in that step (4)
In, the accelerating agent is one or more in two ureas U-24M, UR300 and UR500.
7. the preparation method of high transparency epoxy resin composite material according to claim 1, it is characterised in that step (1)
In, the liquid-state epoxy resin is 3 by mass ratio:1 bisphenol A-type 128 is formed with E51;The solid epoxy resin is by quality
Than being 1:2 bisphenol A-type 901 and 907 forms.
8. the preparation method of high transparency epoxy resin composite material according to claim 1, it is characterised in that step (2)
In, the ultraviolet-resistant aid is 3 by mass ratio:5 UV968 and UV967 composition.
9. the preparation method of high transparency epoxy resin composite material according to claim 1, which is characterized in that step (2)
Described in temperature it is 50 DEG C higher than temperature described in step (3);Temperature described in step (3) is more identical than temperature described in step (4).
10. epoxy prepared by a kind of preparation method by any high transparency epoxy resin composite material described in claim 1-9
Application of the resin composite materials in preparing carbon fiber prepreg.
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Cited By (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN110903602A (en) * | 2019-11-26 | 2020-03-24 | 南京金线金箔总厂 | Preparation and production method of gold foil transparent epoxy resin |
CN111269396A (en) * | 2020-03-27 | 2020-06-12 | 武汉理工大学 | High-light-transmittance oxygen cabin cover prepared from epoxy resin |
CN114058078A (en) * | 2021-12-07 | 2022-02-18 | 江门市严恩化工科技有限公司 | Anti-aging auxiliary agent bag, preparation method and application in carbon fiber prepreg cloth |
Citations (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN104945856A (en) * | 2015-07-14 | 2015-09-30 | 江苏兆鋆新材料股份有限公司 | High-transparency anti-yellowing epoxy resin composite material preparing method and application thereof |
-
2018
- 2018-05-15 CN CN201810458991.6A patent/CN108570217A/en active Pending
Patent Citations (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN104945856A (en) * | 2015-07-14 | 2015-09-30 | 江苏兆鋆新材料股份有限公司 | High-transparency anti-yellowing epoxy resin composite material preparing method and application thereof |
Cited By (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN110903602A (en) * | 2019-11-26 | 2020-03-24 | 南京金线金箔总厂 | Preparation and production method of gold foil transparent epoxy resin |
CN111269396A (en) * | 2020-03-27 | 2020-06-12 | 武汉理工大学 | High-light-transmittance oxygen cabin cover prepared from epoxy resin |
CN114058078A (en) * | 2021-12-07 | 2022-02-18 | 江门市严恩化工科技有限公司 | Anti-aging auxiliary agent bag, preparation method and application in carbon fiber prepreg cloth |
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Application publication date: 20180925 |