CN105440584B - A kind of low shrinkage epoxy resin system and preparation method thereof - Google Patents
A kind of low shrinkage epoxy resin system and preparation method thereof Download PDFInfo
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- CN105440584B CN105440584B CN201510917668.7A CN201510917668A CN105440584B CN 105440584 B CN105440584 B CN 105440584B CN 201510917668 A CN201510917668 A CN 201510917668A CN 105440584 B CN105440584 B CN 105440584B
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- 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
- C08K9/00—Use of pretreated ingredients
- C08K9/04—Ingredients treated with organic substances
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- 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
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/24—Acids; Salts thereof
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- 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
- C08K2201/002—Physical properties
- C08K2201/003—Additives being defined by their diameter
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- 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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- Chemical Kinetics & Catalysis (AREA)
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Abstract
The invention provides a kind of low shrinkage epoxy resin system and preparation method thereof, the low shrinkage epoxy resin system includes each component of following parts by weight：90~110 parts of bisphenol A type epoxy resin, 15~25 parts of epoxide diluent, 40~60 parts of curing agent, 1~3 part of coupling agent, 4~7 parts of nano barium carbonate powder.The low shrinkage epoxy resin that the present invention obtains is compared with bulk resin, and shrinkage factor reduces 50%, while the mechanical property of epoxy resin does not change, can be applied to use in harsh environments, on the structural member that dimensional stability requirements are higher.
Description
Technical field
The present invention relates to a kind of low shrinkage epoxy resin system and preparation method thereof.
Background technology
Epoxy resin is thermosetting tree due to its good caking property, heat resistance, chemical proofing and mechanical performance
A maximum kind of application amount in fat, but cause structure to be received because addition reaction occurs in cross-linking process is solidified for epoxy resin
Contracting, it is certain unfavorable to be brought to the application on the structural member that working environment is severe, dimensional stability requirements are higher, especially
In the structural member of high stable, resin system contraction is excessive to cause structural member type face precision to change, and then influences product
Using effect, it is therefore necessary to reduce the shrinkage factor in epoxy-resin systems solidification process.
The content of the invention
For in the prior art the defects of, it is an object of the invention to provide a kind of low shrinkage epoxy resin system and its preparation
Method.
The purpose of the present invention is achieved through the following technical solutions：
The invention provides a kind of low shrinkage epoxy resin system, it is characterised in that includes each group of following parts by weight
Point：
Preferably, the low shrinkage epoxy resin system includes each component of following parts by weight：
Preferably, the bisphenol A type epoxy resin is E-51 epoxy resin.
Preferably, the average grain diameter of the nano barium carbonate powder is 100~150nm.
Preferably, the coupling agent is titanate esters system coupling agent.
The present invention is surface-treated by coupling agent to barium carbonate powder, improves the dispersion effect of barium titanate.Using receiving
Meter level barium carbonate powder, the shrinkage factor of resin matrix can be reduced when adding less amount.
Preferably, the curing agent is anhydride curing agent；It is furthermore preferred that anhydride curing agent is tetrabydrophthalic anhydride.
Preferably, described epoxide diluent includes butyl glycidyl ether, BDDE, second two
Alcohol diglycidyl ether, phenyl glycidyl ether, polypropylene glycol diglycidyl ether, fatty glycidyl ether, benzyl shrink sweet
Oily ether, 1,6- hexanediol diglycidyl ethers, expoxy propane o-cresyl ether or o-tolyl glycidol ether, neopentyl glycol two
One or more in glycidol ether.Epoxide diluent can reduce epoxy resin solidifying system viscosity, increase mobility.
Present invention also offers a kind of preparation method of low shrinkage epoxy resin system, the preparation method includes following step
Suddenly：
S1, each component parts by weight according to claim 1 weigh raw material；
S2, coupling agent, nano barium carbonate powder be added to stirring reaction in anhydride curing agent, then be ultrasonically treated,
Then obtained reactant a is stood；
S3, it is stirred after bisphenol A type epoxy resin is mixed with epoxide diluent, obtains mixture b；
S4, the reactant a that step S2 is obtained mixed with the mixture b that step S3 is obtained, while be stirred and ultrasound
Processing, produces the low shrinkage epoxy resin system.
Preferably, in step 2, the speed of agitator is 2000~4000 turns/min, and the time is 5~10min；The ultrasound
Processing time is 60~90min；The time of repose is 12~24h.
Preferably, in step 3, the speed of agitator is 2000~4000 turns/min, and the time is 30~60min；Step 4
In, the time of the stirring and supersound process is 60~90min, and speed of agitator is 2000~4000 turns/min.
The present invention improves the dispersion effect of barium titanate, improves metatitanic acid by the mixing of nano barium phthalate and coupling agent
The effect of barium powder, reduce the shrinkage factor of epoxy resin.
Compared with prior art, the present invention has following beneficial effect：
(1) shrinkage factor of the epoxy-resin systems that the present invention obtains in the curing process is low, compared with bulk resin, reduces
50%.
(2) after adding powder, the mechanical property of epoxy resin does not change.
Embodiment
With reference to specific embodiment, the present invention is described in detail.Following examples will be helpful to the technology of this area
Personnel further understand the present invention, but the invention is not limited in any way.It should be pointed out that the ordinary skill to this area
For personnel, without departing from the inventive concept of the premise, various modifications and improvements can be made.These belong to the present invention
Protection domain.
Embodiment 1
A kind of low shrinkage epoxy resin system is present embodiments provided, its each component and parts by weight are as shown in table 1.It is made
Preparation Method comprises the following steps：
Carried out after taking 20 parts of bisphenol A type epoxy resin E-51100 parts, epoxide diluent expoxy propane o-cresyl ether mixing
It is standby after mechanical agitation (2000 turns/min of rotating speed) 30min；
Take 50 parts of tetrabydrophthalic anhydrides, 2 parts of titanate coupling agent, nano barium carbonate powder (average grain diameter 100nm) 5
Part, mechanical agitation 5min after mixing, 24 hours are stood in vacuum drying chamber after then carrying out sonic oscillation 60min；
Ultrasonic vibration 60min is carried out after the above-mentioned two kinds of liquid mixed are mixed while carries out mechanical agitation, has been mixed
It is standby that refrigerator storage is put into after.
Embodiment 2
A kind of low shrinkage epoxy resin system is present embodiments provided, its each component and parts by weight are as shown in table 1.It is made
Preparation Method comprises the following steps：
Machinery is carried out after taking 15 parts of bisphenol A type epoxy resin E-5190 parts, epoxide diluent butyl glycidyl ether mixing
It is standby after stirring (4000 turns/min of rotating speed) 40min；
Take 40 parts of tetrabydrophthalic anhydrides, 1 part of titanate coupling agent, nano barium carbonate powder (average grain diameter 100nm) 4
Part, mechanical agitation 10min after mixing, 18 hours are stood in vacuum drying chamber after then carrying out sonic oscillation 60min；
Ultrasonic vibration 60min is carried out after the above-mentioned two kinds of liquid mixed are mixed while carries out mechanical agitation, has been mixed
It is standby that refrigerator storage is put into after.
Embodiment 3
A kind of low shrinkage epoxy resin system is present embodiments provided, its each component and parts by weight are as shown in table 1.It is made
Preparation Method comprises the following steps：
Machinery is carried out after taking 25 parts of bisphenol A type epoxy resin E-51110 parts, diluent expoxy propane o-cresyl ether mixing
It is standby after stirring (2000 turns/min of rotating speed) 30min；
Take 60 parts of tetrabydrophthalic anhydrides, 3 parts of titanate coupling agent, nano barium carbonate powder (average grain diameter 100nm) 7
Part, mechanical agitation 5min after mixing, 12 hours are stood in vacuum drying chamber after then carrying out sonic oscillation 90min；
Ultrasonic vibration 90min is carried out after the above-mentioned two kinds of liquid mixed are mixed while carries out mechanical agitation, has been mixed
It is standby that refrigerator storage is put into after.
Comparative example 1
This comparative example provides a kind of epoxy-resin systems, and its each component and parts by weight are as shown in table 1.Its preparation method
Comprise the following steps：
Carried out after taking 20 parts of bisphenol A type epoxy resin E-51100 parts, epoxide diluent expoxy propane o-cresyl ether mixing
It is standby after mechanical agitation (2000 turns/min of rotating speed) 30min；
5 parts of 50 parts of tetrabydrophthalic anhydrides, nano barium carbonate powder (average grain diameter 100nm) are taken, machinery stirs after mixing
5min is mixed, 24 hours are stood in vacuum drying chamber after then carrying out sonic oscillation 60min；
Ultrasonic vibration 60min is carried out after the above-mentioned two kinds of liquid mixed are mixed while carries out mechanical agitation, has been mixed
It is standby that refrigerator storage is put into after.
Comparative example 2
This comparative example provides a kind of epoxy-resin systems, and its each component and parts by weight are as shown in table 1.Its preparation method
Comprise the following steps：
Carried out after taking 20 parts of bisphenol A type epoxy resin E-51100 parts, epoxide diluent expoxy propane o-cresyl ether mixing
It is standby after mechanical agitation (2000 turns/min of rotating speed) 30min；
Take 50 parts of tetrabydrophthalic anhydrides, 2 parts of titanate coupling agent, nano barium carbonate powder (average grain diameter 100nm) 2
Part, mechanical agitation 5min after mixing, 24 hours are stood in vacuum drying chamber after then carrying out sonic oscillation 60min；
Ultrasonic vibration 60min is carried out after the above-mentioned two kinds of liquid mixed are mixed while carries out mechanical agitation, has been mixed
It is standby that refrigerator storage is put into after.
Comparative example 3
This comparative example provides a kind of epoxy-resin systems, and its each component and parts by weight are as shown in table 1.Its preparation method
Comprise the following steps：
Carried out after taking 25 parts of bisphenol A type epoxy resin E-51110 parts, epoxide diluent expoxy propane o-cresyl ether mixing
It is standby after mechanical agitation (2000 turns/min of rotating speed) 30min；
Take 60 parts of tetrabydrophthalic anhydrides, 3 parts of titanate coupling agent, nano barium carbonate powder (average grain diameter 100nm) 9
Part, mechanical agitation 5min after mixing, 24 hours are stood in vacuum drying chamber after then carrying out sonic oscillation 60min；
Ultrasonic vibration 60min is carried out after the above-mentioned two kinds of liquid mixed are mixed while carries out mechanical agitation, has been mixed
It is standby that refrigerator storage is put into after.
Comparative example 4
This comparative example provides a kind of epoxy-resin systems, and its each component and parts by weight are as shown in table 1.Its preparation method
Comprise the following steps：
Machinery is carried out after taking 15 parts of bisphenol A type epoxy resin E-5190 parts, epoxide diluent butyl glycidyl ether mixing
It is standby after stirring (4000 turns/min of rotating speed) 40min；
Take 40 parts of tetrabydrophthalic anhydrides, 1 part of titanate coupling agent, nano barium carbonate powder (average grain diameter 100nm) 4
Part, mechanical agitation 30min after mixing, then stand 24 hours in vacuum drying chamber；
Mechanical agitation 60min is carried out after the above-mentioned two kinds of liquid mixed are mixed, refrigerator storage is put into after the completion of mixing
It is standby.
Each component and its parts by weight in the embodiment 1-3 of table 1 and comparative example 1-4
Effect compares：
The testing result of epoxy-resin systems prepared by embodiment 1-3 and comparative example 1-4 is as shown in table 2.
Table 2
The specific embodiment of the present invention is described above.It is to be appreciated that the invention is not limited in above-mentioned
Particular implementation, those skilled in the art can make various deformations or amendments within the scope of the claims, this not shadow
Ring the substantive content of the present invention.
Claims (8)
1. a kind of low shrinkage epoxy resin system, it is characterised in that include each component of following parts by weight：
The average grain diameter of the nano barium carbonate powder is 100nm；
The preparation method of described low shrinkage epoxy resin system comprises the following steps：
S1, according to foregoing each component parts by weight weigh raw material；
S2, coupling agent, nano barium carbonate powder be added to stirring reaction in curing agent, then be ultrasonically treated, then will
The reactant a arrived is stood；
S3, it is stirred after bisphenol A type epoxy resin is mixed with epoxide diluent, obtains mixture b；
S4, the reactant a that step S2 is obtained mixed with the mixture b that step S3 is obtained, while is stirred and is ultrasonically treated,
Produce the low shrinkage epoxy resin system.
2. low shrinkage epoxy resin system as claimed in claim 1, it is characterised in that include each group of following parts by weight
Point：
3. low shrinkage epoxy resin system as claimed in claim 1, it is characterised in that the bisphenol A type epoxy resin is E-
51 epoxy resin.
4. low shrinkage epoxy resin system as claimed in claim 1, it is characterised in that the coupling agent is coupled for titanate esters system
Agent.
5. low shrinkage epoxy resin system as claimed in claim 1, it is characterised in that the curing agent solidifies for anhydrides
Agent.
6. low shrinkage epoxy resin system as claimed in claim 1, it is characterised in that described epoxide diluent includes phenyl
One or more in glycidol ether, fatty glycidyl ether, benzyl glycidyl ether, expoxy propane o-cresyl ether.
7. low shrinkage epoxy resin system as claimed in claim 1, it is characterised in that in step S2, the speed of agitator is
2000~4000 turns/min, the time is 5~10min；The sonication treatment time is 60~90min；The time of repose is 12
~24h.
8. low shrinkage epoxy resin system as claimed in claim 1, it is characterised in that in step S3, the speed of agitator is
2000~4000 turns/min, the time is 30~60min；In step S4, time of the stirring and supersound process for 60~
90min, speed of agitator are 2000~4000 turns/min.
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| CN201510917668.7A CN105440584B (en) | 2015-12-10 | 2015-12-10 | A kind of low shrinkage epoxy resin system and preparation method thereof |
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| CN109880565A (en) * | 2019-03-12 | 2019-06-14 | 中国石油大学(华东) | A kind of limestone deep-well stabilizing borehole rubber plug and preparation method thereof |
| CN111825954A (en) * | 2020-06-30 | 2020-10-27 | 上海复合材料科技有限公司 | Normal-temperature curing resin system for copying antenna reflecting surface and preparation method thereof |
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|---|---|---|---|---|
| CN103865234A (en) * | 2014-04-08 | 2014-06-18 | 上海交通大学 | Preparation method of micro/nano inorganic particle/epoxy resin ternary composites |
| CN104292764A (en) * | 2014-10-31 | 2015-01-21 | 常熟市微尘电器有限公司 | Composite dielectric material for high energy-storage capacitor and preparation method of composite dielectric material |
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| CN101747593B (en) * | 2009-11-19 | 2011-08-10 | 哈尔滨工业大学 | Conductive adhesive with barium titanate ceramic powder as conductive filler and preparation method thereof |
| CN103030926B (en) * | 2011-09-30 | 2016-08-31 | 深圳光启高等理工研究院 | A kind of preparation method of medium substrate |
| CN103387736A (en) * | 2012-05-11 | 2013-11-13 | 富葵精密组件(深圳)有限公司 | Epoxy resin composite material and preparation method thereof |
| KR101926808B1 (en) * | 2012-12-28 | 2018-12-07 | 삼성전기주식회사 | Resin composition with good workability, insulating film, and prepreg |
| JP2014232249A (en) * | 2013-05-30 | 2014-12-11 | 株式会社Adeka | Photosensitive composition |
| CN103965589B (en) * | 2014-05-14 | 2016-08-31 | 武汉理工大学 | A kind of piezo-electric damping polymer vibration isolation pad and preparation method thereof |
| CN104974468B (en) * | 2015-03-31 | 2017-05-17 | 合复新材料科技(无锡)有限公司 | Thermosetting laser-induced metallization thermal-conduction composite material with stable high dielectric constant |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103865234A (en) * | 2014-04-08 | 2014-06-18 | 上海交通大学 | Preparation method of micro/nano inorganic particle/epoxy resin ternary composites |
| CN104292764A (en) * | 2014-10-31 | 2015-01-21 | 常熟市微尘电器有限公司 | Composite dielectric material for high energy-storage capacitor and preparation method of composite dielectric material |
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