CN107540818A - A kind of high-performance modified epoxy acrylic resin and preparation method thereof - Google Patents
A kind of high-performance modified epoxy acrylic resin and preparation method thereof Download PDFInfo
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- CN107540818A CN107540818A CN201710626521.1A CN201710626521A CN107540818A CN 107540818 A CN107540818 A CN 107540818A CN 201710626521 A CN201710626521 A CN 201710626521A CN 107540818 A CN107540818 A CN 107540818A
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Abstract
The invention discloses a kind of high-performance modified epoxy acrylic resin and preparation method thereof, it is made up of the component of following parts by weight：40~80 parts of bisphenol A type epoxy resin, 20~45 parts of caprolactone modification acrylate, 15~45 parts of acid anhydrides, 0.5~5 part of catalyst, 0.01~2 part of polymerization inhibitor, 80~150 parts of pentaerythritol triacrylate.The modified epoxy of the present invention not only increases the original performance of resin, and greatly improves its toughness.Its relative viscosity is low, improve the convenience used, cheaper, improve economy, available in Primer for Vacuum Plating of Plastics, finish paint, upper plating, the adhesive force to base material and the wettability to ground of priming paint can be improved, for various chemical resistances can be improved in finish paint, the polyurethane resin of costliness can be replaced with it.
Description
Technical field
The invention belongs to light-cured resin field, and in particular to a kind of high-performance modified epoxy acrylic resin.
Background technology
Epoxy acrylate（EA）It is a kind of light-cured resin that dosage is maximum in solidification field, its cohesiveness is high, solidification
Speed is fast, wetability is good, compatibility is good, glossiness is high, chemical resistance is excellent, and raw material is easy to get, is cheap, quilt
It is widely used in the industries such as adhesive, coating and ink.But also there is the curing agent or solid that fragility is big, weatherability is poor, traditional in EA
The problems such as universal color of change system is deep, the big bond strength between low-surface-energy material of smell is small, therefore for problem above to it
Being modified research turns into study hotspot.
Epoxy acrylate common method of modifying last year includes that fatty acid modified, amine is modified, Si modification, acid anhydrides change at present
Property, P Modification, polyamine are ester modified etc., and these EA modification technologies achieve major progress, various modified epoxies third in some aspects
Olefin(e) acid resin sticks agent, ink, coating and composite industry in ultraviolet cured adhesive and obtains extensive use.It is but a kind of modified
Method can only often improve EA performance in a certain respect, and the otherwise advantage of regular weakening.
The content of the invention
The purpose of the present invention is on the basis of existing technology, there is provided a kind of high-performance modified epoxy acrylic resin.
It is a further object of the present invention to provide a kind of preparation method of above-mentioned high-performance modified epoxy acrylic resin.
The purpose of the present invention can be reached by following measures：
A kind of high-performance modified epoxy acrylic resin, it is made up of the component of following parts by weight：Bisphenol A type epoxy resin 40~
80 parts, 20~45 parts of caprolactone modification acrylate, 15~45 parts of acid anhydrides, 0.5~5 part of catalyst, 0.01~2 part of polymerization inhibitor,
80~150 parts of pentaerythritol triacrylate.
In a kind of preferred scheme, this modified epoxy acrylate resin is made up of the component of following parts by weight：Bisphenol-A type ring
45~75 parts of oxygen tree fat, 30~45 parts of caprolactone modification acrylate, 20~45 parts of acid anhydrides, 1~5 part of catalyst, polymerization inhibitor
0.01~1 part, 80~120 parts of pentaerythritol triacrylate.
In a kind of preferred scheme, this modified epoxy acrylate resin is made up of the component of following parts by weight：Bisphenol-A type ring
50~70 parts of oxygen tree fat, 30~40 parts of caprolactone modification acrylate, 20~40 parts of acid anhydrides, 1~5 part of catalyst, polymerization inhibitor
0.01~1 part, 90~110 parts of pentaerythritol triacrylate.
In a kind of more preferably scheme, this modified epoxy acrylate resin is made up of the component of following parts by weight：Bisphenol A-type
56~65 parts of epoxy resin, 30~40 parts of caprolactone modification acrylate, 25~35 parts of acid anhydrides, 1~5 part of catalyst, polymerization inhibitor
0.01~1 part, 5~110 parts of pentaerythritol triacrylate.
Polymerization inhibitor in the present invention is MEHQ, and catalyst is TBAB.
A kind of preparation method of above-mentioned high-performance modified epoxy acrylic resin, it comprises the following steps：
（1）After pentaerythritol triacrylate and caprolactone acrylate are mixed in proportion, a part of polymerization inhibitor mixing is added
Uniformly, 70~90 DEG C are heated to, acid anhydrides is added and carries out compound of the ring-opening reaction generation with carboxyl, obtain reaction intermediate
1；
（2）By being mixed and heated to 90~110 DEG C for bisphenol A type epoxy resin and another part polymerization inhibitor, by the intermediate 1
Mix with catalyst, then mixed with the mixture containing epoxy resin, while control temperature to be reacted at 90~110 DEG C.
In step（1）In, it is preferred that the temperature of ring-opening reaction is 80 DEG C；The polymerization inhibitor used in the step accounts for polymerization inhibitor
The 60~80% of total amount.
In step（2）In, it is preferred that reaction carries out stopping reaction when being less than 5mgKOH/g to measure material acid number.Bisphenol-A
Type epoxy resin and another part polymerization inhibitor are mixed and heated to 100 DEG C；Reaction temperature is 100 ± 2 DEG C.
Epoxy acrylate is a kind of light-cured resin that dosage is maximum in solidification field, and its cohesiveness is high, curing rate
Hurry up, wetability is good, compatibility is good, glossiness is high, endurance is excellent, and raw material is easy to get, is cheap, being widely used, still
There is also this big fatal defects of this fragility for it.And the modified epoxy that this is done not only increases its original property
Can, and greatly improve its toughness.And compared to polyurethane-modified epoxy acrylic resin, what this was done
Resin relative viscosity is low, improves the convenience used, cheaper, improves economy, but similar to its performance.Can
For upper plating, the adhesive force to base material and the profit to ground of priming paint in Primer for Vacuum Plating of Plastics, finish paint, can be improved
Wet performance, for various chemical resistances can be improved in finish paint, the polyurethane resin of costliness can be replaced with it.
Embodiment
Present disclosure is described further with reference to embodiments, but protection scope of the present invention is not limited to
Following embodiment.
Embodiment 1
After pentaerythritol triacrylate 106g and 36g caprolactone acrylate is mixed in proportion, add 0.17g polymerization inhibitors and mix
Close uniformly, be heated to 80 DEG C, add 30g acid anhydrides and carry out compound of the ring-opening reaction generation with carboxyl, be reacted to theoretical acid
Value, will obtain reaction intermediate 1；
By being mixed and heated to 100 DEG C for 60g bisphenol A type epoxy resins and 0.06g polymerization inhibitors, by the intermediate 1 and 1.8g
Catalyst mixes, and is then mixed with the mixture containing epoxy resin, while control temperature to be reacted at 100 DEG C.Reaction is carried out
Stop reaction when being less than 5mgKOH/g to measure material acid number, obtain high-performance modified epoxy acrylic resin.Its main performance
It is shown in Table 1.
Embodiment 2
After pentaerythritol triacrylate 100g and 33g caprolactone acrylate is mixed in proportion, add 0.15g polymerization inhibitors and mix
Close uniformly, be heated to 80 DEG C, add 28g acid anhydrides and carry out compound of the ring-opening reaction generation with carboxyl, be reacted to theoretical acid
Value, will obtain reaction intermediate 1；
By being mixed and heated to 100 DEG C for 63g bisphenol A type epoxy resins and 0.06g polymerization inhibitors, by the intermediate 1 and 1.7g
Catalyst mixes, and is then mixed with the mixture containing epoxy resin, while control temperature to be reacted at 100 DEG C.Reaction is carried out
Stop reaction when being less than 5mgKOH/g to measure material acid number, obtain high-performance modified epoxy acrylic resin.Its main performance
It is shown in Table 1.
Embodiment 3
After pentaerythritol triacrylate 112g and 37g caprolactone acrylate is mixed in proportion, add 0.18g polymerization inhibitors and mix
Close uniformly, be heated to 80 DEG C, add 30g acid anhydrides and carry out compound of the ring-opening reaction generation with carboxyl, be reacted to theoretical acid
Value, will obtain reaction intermediate 1；
By being mixed and heated to 100 DEG C for 63g bisphenol A type epoxy resins and 0.06g polymerization inhibitors, by the intermediate 1 and 1.8g
Catalyst mixes, and is then mixed with the mixture containing epoxy resin, while control temperature to be reacted at 100 DEG C.Reaction is carried out
Stop reaction when being less than 5mgKOH/g to measure material acid number, obtain high-performance modified epoxy acrylic resin.Its main performance
It is shown in Table 1.
The performance test of embodiment 4
Epoxy acrylic resin base-material obtained by each embodiment is smeared on the glass sheet, then sheet glass is put into 18 volts of uviol lamps and shone
Penetrate, lamp is away from for 15 centimetres, until cured film reaches surface drying, hardening time is less than 15 minutes, that is, obtains cured film.By testing,
The solidification film hardness is tested according to GB/T6739-1996 " hardness of paint film pencil determination method ", adhesive force is according to GB/T9286-
1998 standards are measured as 3, and correlated performance see the table below.
The main performance of the high-performance modified epoxy acrylic resin of the present invention of table 1
Comparative example 1
Caprolactone acrylate in embodiment 1 is changed to acrylate, other are the same as embodiment 1.Obtained epoxy acrylic tree
For the viscosity (25 DEG C) of fat in more than 30000mpa.s, toughness 1mm film crackings have breakage, and hardening time is more than 25 minutes.
Claims (9)
1. a kind of high-performance modified epoxy acrylic resin, it is characterised in that it is made up of the component of following parts by weight：Bisphenol A-type
40~80 parts of epoxy resin, 20~45 parts of caprolactone modification acrylate, 15~45 parts of acid anhydrides, 0.5~5 part of catalyst, inhibition
0.01~2 part of agent, 80~150 parts of pentaerythritol triacrylate.
2. high-performance modified epoxy acrylic resin according to claim 1, it is characterised in that it is by following parts by weight
Component is made：45~75 parts of bisphenol A type epoxy resin, 30~45 parts of caprolactone modification acrylate, 20~45 parts of acid anhydrides, catalysis
1~5 part of agent, 0.01~1 part of polymerization inhibitor, 80~120 parts of pentaerythritol triacrylate.
3. high-performance modified epoxy acrylic resin according to claim 2, it is characterised in that it is by following parts by weight
Component is made：50~70 parts of bisphenol A type epoxy resin, 30~40 parts of caprolactone modification acrylate, 20~40 parts of acid anhydrides, catalysis
1~5 part of agent, 0.01~1 part of polymerization inhibitor, 90~110 parts of pentaerythritol triacrylate.
4. high-performance modified epoxy acrylic resin according to claim 3, it is characterised in that it is by following parts by weight
Component is made：56~65 parts of bisphenol A type epoxy resin, 30~40 parts of caprolactone modification acrylate, 25~35 parts of acid anhydrides, catalysis
1~5 part of agent, 0.01~1 part of polymerization inhibitor, 5~110 parts of pentaerythritol triacrylate.
5. the high-performance modified epoxy acrylic resin according to Claims 1 to 4 any one, it is characterised in that the resistance
Poly- agent is MEHQ, and catalyst is TBAB.
6. the preparation method of high-performance modified epoxy acrylic resin described in claim 1, it is characterised in that comprise the following steps：
（1）After pentaerythritol triacrylate and caprolactone acrylate are mixed in proportion, a part of polymerization inhibitor mixing is added
Uniformly, 70~90 DEG C are heated to, acid anhydrides is added and carries out compound of the ring-opening reaction generation with carboxyl, obtain reaction intermediate
1；
（2）By being mixed and heated to 90~110 DEG C for bisphenol A type epoxy resin and another part polymerization inhibitor, by the intermediate 1
Mix with catalyst, then mixed with the mixture containing epoxy resin, while control temperature to be reacted at 90~110 DEG C.
7. the preparation method of high-performance modified epoxy acrylic resin according to claim 6, it is characterised in that in step
（1）In, the temperature of ring-opening reaction is 80 DEG C；The polymerization inhibitor used in the step accounts for the 60~80% of polymerization inhibitor total amount.
8. the preparation method of high-performance modified epoxy acrylic resin according to claim 6, it is characterised in that in step
（2）In, reaction carries out stopping reaction when being less than 5mgKOH/g to measure material acid number.
9. the preparation method of high-performance modified epoxy acrylic resin according to claim 6, it is characterised in that in step
（2）In, bisphenol A type epoxy resin and another part polymerization inhibitor are mixed and heated to 100 DEG C；Reaction temperature is 100 ± 2 DEG C.
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| CN201710626521.1A CN107540818A (en) | 2017-07-27 | 2017-07-27 | A kind of high-performance modified epoxy acrylic resin and preparation method thereof |
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1143086A (en) * | 1995-04-13 | 1997-02-19 | 三井东压化学株式会社 | Epoxy propenoic acid resin and its use |
| CN101449325A (en) * | 2006-05-24 | 2009-06-03 | Dic株式会社 | Optical disk and ultraviolet-curable composition for optical disk |
| CN102385250A (en) * | 2011-06-29 | 2012-03-21 | 南昌大学 | Ultraviolet laser solidification rapid-prototyping photosensitive resin and manufacture method thereof |
| CN101906268B (en) * | 2010-03-15 | 2012-09-26 | 湖南松井新材料有限公司 | Coating composite and optical fiber containing same |
| CN105255353A (en) * | 2015-10-09 | 2016-01-20 | 安徽嘉年华漆业有限公司 | High-strength impact resistance oil paint |
-
2017
- 2017-07-27 CN CN201710626521.1A patent/CN107540818A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1143086A (en) * | 1995-04-13 | 1997-02-19 | 三井东压化学株式会社 | Epoxy propenoic acid resin and its use |
| CN101449325A (en) * | 2006-05-24 | 2009-06-03 | Dic株式会社 | Optical disk and ultraviolet-curable composition for optical disk |
| CN101906268B (en) * | 2010-03-15 | 2012-09-26 | 湖南松井新材料有限公司 | Coating composite and optical fiber containing same |
| CN102385250A (en) * | 2011-06-29 | 2012-03-21 | 南昌大学 | Ultraviolet laser solidification rapid-prototyping photosensitive resin and manufacture method thereof |
| CN105255353A (en) * | 2015-10-09 | 2016-01-20 | 安徽嘉年华漆业有限公司 | High-strength impact resistance oil paint |
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