CN108485198A - A kind of high dielectric property mould material - Google Patents
A kind of high dielectric property mould material Download PDFInfo
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- CN108485198A CN108485198A CN201810328399.4A CN201810328399A CN108485198A CN 108485198 A CN108485198 A CN 108485198A CN 201810328399 A CN201810328399 A CN 201810328399A CN 108485198 A CN108485198 A CN 108485198A
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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
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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
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
- C08K2003/2227—Oxides; Hydroxides of metals of aluminium
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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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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/02—Flame or fire retardant/resistant
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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
- C08L2201/00—Properties
- C08L2201/08—Stabilised against heat, light or radiation or oxydation
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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
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Abstract
The present invention relates to a kind of high dielectric property mould material, preparation method includes that high dielectric filler is added in difunctional epoxy systems, and 130 DEG C are stirred 20 minutes, then at 95 DEG C, simple function group epoxy systems, nano alumina particles are added, stirs 130 minutes, obtains glue；It will be added in mold after glue vacuum defoamation, then after hot-press solidifying, obtain high dielectric property mould material, protruded with excellent flame retardant property, heat resistance, especially dielectric constant.
Description
Technical field
The invention belongs to electronics technical field of composite materials, and in particular to a kind of high dielectric property mould material.
Background technology
With the continuous development of science and technology, the application of polymer-based composite is more and more extensive.Meanwhile each application
Also to different materials, more stringent requirements are proposed accordingly in field, such as high temperature resistant, resistance to ablation, high dielectric etc..Due to for
Size is miniaturized and the further demand of high energy storage density, and huge dielectric constant material is always modern capacitor, filter
The hot spot of equal electronic devices research.With fire-retardant attention, it is desirable that product has flame retardant property, fire-retardant to have class requirement,
Respectively UL94 V-2, UL94 V-1 and UL94 V-0 ranks, wherein UL94 V-0 ranks are whether existing judgement substance hinders
The international standard of combustion.Equalization point is found between fire prevention and environmental protection, is the important node of the following flame retardant products development.Fire retardant exists
Importance in modern society can not be ignored, but as a series of environmental protection policies in Europe are put into effect, development and application is to some extent
It is restricted.How while support personnel and property are from fire threat, and fire retardant can be made to deposit human body and environment
Potential hazard be preferably minimized, be electrical domestic fire retardant manufacturing enterprise, research institution and downstream electronic, building materials, traffic and
The common focus of attention of the industries such as furniture.Using complex technique, the advantages of being not only to integrate organic-inorganic material, compatibility is also wanted not
Same organic component, is hopeful to prepare the material for meeting commercial Application.
Invention content
The object of the present invention is to provide a kind of high dielectric property mould materials, have excellent dielectric properties, excellent is resistance to
Hot, anti-flammability, processability and mechanical property；Our company has applied for multiple patents together simultaneously, illustrates from different directions
Central inventive point, it is especially longitudinal deep, it is expected that obtaining comprehensive protection.
To achieve the above object of the invention, the technical solution adopted by the present invention is：
A kind of high dielectric property mould material, preparation method includes the following steps：
(1) six water manganese nitrates, cobalt nitrate hexahydrate and iron chloride are scattered in deionized water, 45 is stirred at 110 DEG C
Minute, obtain presoma system；Then filtering presoma system obtains presoma；Then presoma passed through into drying, calcined
To high dielectric filler；The drying is the lower 105 DEG C of dryings of vacuum；The calcining is under hydrogen/argon gas mixed atmosphere, and 1150 DEG C are forged
It burns 3 hours；The volume ratio of the hydrogen/argon gas is 0.5: 10；
(2) at room temperature, 3,3 '-dithiodipropionic acids, dichloromethane, acetone are mixed；Then m-nitrobenzene sulfonic acid pyrrole is added
Methyl butynol is added in pyridine salt and diphenyl phosphate, stirring after ten minutes, and stirring adds 2,3- epoxies basic ring penta after 35 minutes
Benzylidene aniline is added after 50 minutes in cyclopentyl ether, stirring, continues stirring 5 minutes；Then N is added, N '-dicyclohexyls carbon two is sub-
Amine continues stirring 30 minutes, obtains simple function group epoxy systems；
(3) -2 propyl alcohol of 2- methyl is mixed to addition phthalic acid two after ten minutes to contract with isomery undecyl alcohol polyoxyethylene ether
In water glyceride, 125 DEG C are stirred 5 minutes, and polyetherimide is then added, and are continued stirring 45 minutes, are obtained difunctional epoxy
System；
(4) high dielectric filler is added in difunctional epoxy systems, 130 DEG C are stirred 20 minutes, then at 95 DEG C, are added
Enter simple function group epoxy systems, nano alumina particles, stirs 130 minutes, obtain glue；
(5) it will be added in mold after glue vacuum defoamation, then after hot-press solidifying, obtain high dielectric property mould material.
In above-mentioned technical proposal, in step (1), the six water manganese nitrate, cobalt nitrate hexahydrate, iron chloride mass ratio be 1:
1∶0.2。
In above-mentioned technical proposal, in step (2), 3,3 '-dithiodipropionic acids, dichloromethane, acetone, m-nitrobenzene sulfonic acid
Pyridiniujm, diphenyl phosphate, methyl butynol, 2,3- epoxy group cyclopenta rings amyl ether, benzylidene aniline, N, N '-dicyclohexyls
The mass ratio of carbodiimide is 0.005: 0.15: 1: 0.002: 0.2: 0.02: 1: 0.3: 0.05；Be added methyl butynol when
Between be 20 minutes.
In above-mentioned technical proposal, in step (3), -2 propyl alcohol of 2- methyl, isomery undecyl alcohol polyoxyethylene ether, phthalic acid
2-glycidyl ester, polyetherimide mass ratio be 0.2: 0.1: 1: 0.09.
In above-mentioned technical proposal, in step (4), high dielectric filler, difunctional epoxy systems, simple function group epoxy body
It is, the mass ratio of nano alumina particles is 0.09: 0.4: 1: 0.01.
In above-mentioned technical proposal, in step (5), the temperature of vacuum defoamation is 90 DEG C, and the time is 10 minutes, and vacuum degree is
1KPa；The condition of hot-press solidifying is 2kg/cm2/130℃/20min+5kg/cm2/160℃ /30min++8kg/cm2/190℃/
50min+8kg/cm2/ 210 DEG C/10min+ Temperature falls.This is critically important for the present invention, makes material abundant under vacuum conditions
Degassing just can guarantee that product high reliability request also avoids pre-polymerization excessive, especially ensure stabilization of the filler in hot-press solidifying
Property, the dispersibility of filler is good with compatibility, while the adjustment viscosity provided using minute quantity nano alumina particles with it is compatible
The effect of property, reaches good dispersion effect.For the present invention by whole compatibility and technological design, obtained epoxy material is heat-resisting very
It is good, fire-retardant very well, hydroscopicity it is low, especially dielectric constant performance is good.Inventor develops cooperatively with school, and creative utilizes hydrogen
Gas argon gas mixed gas calcination processing so that Lacking oxygen increases inside filler, more free electrons is produced, in conjunction with small molecule
Compound is directly used in resin compounded system and is conducive to participate in the solidification process of resin, is on the one hand adjusted and is filled out by several organic molecular species
The surface nature of material, preventing inorganic particulate, it generates the too fast influence of partial polymerization to resin, in addition it can adjust polymer
Cross-linked network so that cured product crosslinking is reasonable, and it is excessive to be unlikely to brittleness, to which conducive to processing, 1.5 millimeters of feeds fishing sides reach
57 meters.The present invention is mixed with several compound pre-reactions first before epoxy is added, high so as to be accessed with epoxy reaction
Molecular backbone can also improve wet-heat resisting fire-retardant while will not reduce heat-resisting.The present invention simple function group epoxy and difunctionality
Group does not use conventional four-functional group epoxy, still heat-resisting good, also improves processability.
The present invention does not use fire retardant, by modified filler and compound effects, is imitated in combination with polymer reaction
Fruit, material can form finer and close protective layer in heated and burning, reach excellent hot oxygen screen effect, solid to assign
Body adhesives excellent heat resistance and anti-flammability, while mechanical property, adhesive property are good；Overcome the resistance of prior art filler
Mechanical properties decrease, the problem of heat-resisting decline that the bonding that combustion agent is brought declines and reactive flame retardant is brought.
Since above-mentioned technical proposal is used, the present invention has following advantages compared with prior art：
Compound system composition provided by the invention is reasonable, then prepares technique, inorganic nanoparticles in obtained base material
There is uniform dispersion degree, preparation process to belong to chemical process in system, the inorganic matter of formation is combined with the surface of interlaminar resin
Power is much stronger than the surface binding force of traditional physical mechanical blending.The material system composition that the present invention utilizes is reasonable, each to form
/ compatibility is good, and high dielectric property mould material has thus been prepared, and has good mechanical property, heat resistance, comprehensive
The shortcomings that the advantages of closing polymer, two component of inorganic particulate, two component of improvement, obtains the comprehensive performance of material to improve；Gu
Change effect is good, and cross-linked structure is uniform, on the one hand micromolecular compound can increase system as the compatilizer of macromolecule organic
On the other hand the compatibility of each component avoids forming crosslinking uneven defect when hot-press solidifying, ensures that resin system forms stabilization
Structure, especially improve heat-resisting, the wearability of conventional epoxy, and be free of fire retardant, pass through reasonable reaction, success
The hygroscopic defect of existing reactive phosphor-containing flame-proof molecule is avoided, unexpected effect is achieved.
Specific implementation mode
With reference to embodiment, the invention will be further described：
Embodiment one
A kind of high dielectric property mould material, preparation method includes the following steps：
(1) six water manganese nitrates, cobalt nitrate hexahydrate and iron chloride are scattered in deionized water, 45 is stirred at 110 DEG C
Minute, obtain presoma system；Then filtering presoma system obtains presoma；Then presoma passed through into drying, calcined
To high dielectric filler；The drying is the lower 105 DEG C of dryings of vacuum；The calcining is under hydrogen/argon gas mixed atmosphere, and 1150 DEG C are forged
It burns 3 hours；The volume ratio of the hydrogen/argon gas is 0.5: 10；
(2) at room temperature, 3,3 '-dithiodipropionic acids, dichloromethane, acetone are mixed；Then m-nitrobenzene sulfonic acid pyrrole is added
Methyl butynol is added in pyridine salt and diphenyl phosphate, stirring after ten minutes, and stirring adds 2,3- epoxies basic ring penta after 35 minutes
Benzylidene aniline is added after 50 minutes in cyclopentyl ether, stirring, continues stirring 5 minutes；Then N is added, N '-dicyclohexyls carbon two is sub-
Amine continues stirring 30 minutes, obtains simple function group epoxy systems；
(3) -2 propyl alcohol of 2- methyl is mixed to addition phthalic acid two after ten minutes to contract with isomery undecyl alcohol polyoxyethylene ether
In water glyceride, 125 DEG C are stirred 5 minutes, and polyetherimide is then added, and are continued stirring 45 minutes, are obtained difunctional epoxy
System；
(4) high dielectric filler is added in difunctional epoxy systems, 130 DEG C are stirred 20 minutes, then at 95 DEG C, are added
Enter simple function group epoxy systems, nano alumina particles, stirs 130 minutes, obtain glue；
(5) it will be added in mold after glue vacuum defoamation, then after hot-press solidifying, obtain high dielectric property mould material,
The temperature of 3.8 millimeters of thickness, vacuum defoamation is 90 DEG C, and the time is 10 minutes, vacuum degree 1KPa；The condition of hot-press solidifying is
2kg/cm2/130℃/20min+5kg/cm2/160℃ /30min++8kg/cm2/190℃/50min+8kg/cm2/210℃/
10min+ Temperature falls.
In step (1), six water manganese nitrates, cobalt nitrate hexahydrate, iron chloride mass ratio be 1: 1: 0.2；In step (2), 3,
3 '-dithiodipropionic acids, dichloromethane, acetone, m-nitrobenzene sulfonic acid pyridiniujm, diphenyl phosphate, methyl butynol, 2,3- rings
The mass ratio of oxygroup cyclopenta ring amyl ether, benzylidene aniline, N, N '-dicyclohexylcarbodiimides are 0.005: 0.15: 1: 0.002
∶0.2∶0.02∶1∶0.3∶0.05；The time that methyl butynol is added is 20 minutes；In step (3), -2 propyl alcohol of 2- methyl, isomery
Undecyl alcohol polyoxyethylene ether, o-phthalic acid diglycidyl ester, polyetherimide mass ratio be 0.2: 0.1: 1: 0.09；
In step (4), high dielectric filler, difunctional epoxy systems, simple function group epoxy systems, nano alumina particles mass ratio
It is 0.09: 0.4: 1: 0.01.
Comparative example one
As embodiment one, the wherein calcining of step (1) is under argon gas atmosphere, and 1150 DEG C are calcined 3 hours.
Comparative example two
As embodiment one, wherein step (2) is added without diphenyl phosphate.
Comparative example three
As embodiment one, wherein step (3) is added without polyetherimide.
Comparative example four
As embodiment one, wherein step (4) is added without nano alumina particles.
To mechanical performance (unnotched impact strength, the Kj/m of the plank in above-described embodiment and comparative example2), mechanical property
Can (1.5 millimeters of feeds, rice), hot property, dielectric constant (1MHz), water absorption rate, it is fire-retardant be determined, as a result referring to table 1.
The performance of 1 high dielectric property mould material of table
| It is fire-retardant | Oxygen index (OI) | Drag for side | Dielectric constant | Tg/℃ | Hydroscopicity | Impact strength | |
| Embodiment one | V0 | 40 | 128 | 99 | 221 | 0.051% | 5.6 |
| Comparative example one | V0 | 40 | 120 | 26 | 217 | 0.051% | 5.1 |
| Comparative example two | V1 | 22 | 117 | 96 | 192 | 0.058% | 4.8 |
| Comparative example three | V0 | 28 | 101 | 83 | 190 | 0.062% | 4.6 |
| Comparative example four | V1 | 24 | 105 | 81 | 201 | 0.061% | 4.5 |
To sum up, high dielectric property mould material composition disclosed by the invention is reasonable, and compatibility is good between each component, thus
High dielectric property mould material has been prepared, there is good flame retardant property, excellent heat resistance, especially there is low suction
Wet rate and good dielectric properties.
Claims (7)
1. a kind of high dielectric property mould material, which is characterized in that preparation method includes the following steps：
(1) six water manganese nitrates, cobalt nitrate hexahydrate and iron chloride are scattered in deionized water, are stirred 45 minutes at 110 DEG C,
Obtain presoma system；Then filtering presoma system obtains presoma；Then presoma is obtained into Gao Jie by dry, calcining
Electric filler；The drying is the lower 105 DEG C of dryings of vacuum；The calcining is under hydrogen/argon gas mixed atmosphere, and 1150 DEG C of calcinings 3 are small
When；The volume ratio of the hydrogen/argon gas is 0.5: 10；
(2) at room temperature, 3,3 '-dithiodipropionic acids, dichloromethane, acetone are mixed；Then m-nitrobenzene sulfonic acid pyridiniujm is added
With diphenyl phosphate, methyl butynol is added in stirring after ten minutes, and stirring adds 2,3- epoxy group cyclopenta rings after 35 minutes
Benzylidene aniline is added after 50 minutes in amyl ether, stirring, continues stirring 5 minutes；Then it is added N, N '-dicyclohexylcarbodiimides,
Continue stirring 30 minutes, obtains simple function group epoxy systems；
(3) -2 propyl alcohol of 2- methyl is mixed with isomery undecyl alcohol polyoxyethylene ether after ten minutes be added phthalic acid two shrink it is sweet
In grease, 125 DEG C are stirred 5 minutes, and polyetherimide is then added, and are continued stirring 45 minutes, are obtained difunctional epoxy systems；
(4) high dielectric filler is added in difunctional epoxy systems, 130 DEG C are stirred 20 minutes, then at 95 DEG C, are added single
Functional group's epoxy systems, nano alumina particles stir 130 minutes, obtain glue；
(5) it will be added in mold after glue vacuum defoamation, then after hot-press solidifying, obtain high dielectric property mould material.
2. high dielectric property mould material according to claim 1, it is characterised in that：In step (1), the six water nitric acid
Manganese, cobalt nitrate hexahydrate, iron chloride mass ratio be 1: 1: 0.2.
3. high dielectric property mould material according to claim 1, it is characterised in that：In step (2), 3,3 '-two thio two
Propionic acid, dichloromethane, acetone, m-nitrobenzene sulfonic acid pyridiniujm, diphenyl phosphate, methyl butynol, 2,3- epoxy cyclopentyls
The mass ratio of cyclopenta ether, benzylidene aniline, N, N '-dicyclohexylcarbodiimides are 0.005: 0.15: 1: 0.002: 0.2: 0.02:
1∶0.3∶0.05；The time that methyl butynol is added is 20 minutes.
4. high dielectric property mould material according to claim 1, it is characterised in that：In step (3), -2 propyl alcohol of 2- methyl,
Isomery undecyl alcohol polyoxyethylene ether, o-phthalic acid diglycidyl ester, polyetherimide mass ratio be 0.2: 0.1: 1:
0.09。
5. high dielectric property mould material according to claim 1, it is characterised in that：It is high dielectric filler, double in step (4)
Functional group's epoxy systems, simple function group epoxy systems, nano alumina particles mass ratio be 0.09: 0.4: 1: 0.01.
6. high dielectric property mould material according to claim 1, it is characterised in that：In step (5), the temperature of vacuum defoamation
It it is 90 DEG C, the time is 10 minutes, vacuum degree 1KPa.
7. high dielectric property mould material according to claim 1, it is characterised in that：In step (5), the condition of hot-press solidifying
For 2kg/cm2/130℃/20min+5kg/cm2/160℃/30min++8kg/cm2/190℃/50min+8kg/cm2/210℃/
10min+ Temperature falls.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810116690 | 2018-01-27 | ||
| CN2018101166905 | 2018-01-27 |
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| Publication Number | Publication Date |
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| CN201810328399.4A Withdrawn CN108485198A (en) | 2018-01-27 | 2018-04-04 | A kind of high dielectric property mould material |
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Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101037225A (en) * | 2007-02-06 | 2007-09-19 | 南京航空航天大学 | Titanium dioxide nano thread, belt and tube block array and preparation method thereof |
| CN101659805A (en) * | 2009-09-24 | 2010-03-03 | 同济大学 | Preparation method of composite wave absorbing powder with wide frequency band |
| CN104370285A (en) * | 2014-10-23 | 2015-02-25 | 北京大学 | Method for macroscopically preparing high-quality graphene by using bio-mineralized material |
| CN105086448A (en) * | 2015-08-31 | 2015-11-25 | 苏州凯欧曼新材料科技有限公司 | High-dielectric constant composite material |
| CN105172297A (en) * | 2015-09-02 | 2015-12-23 | 苏州益可泰电子材料有限公司 | Flame-resistant and heat-resistant copper clad laminate preparation method |
| CN106449145A (en) * | 2016-11-08 | 2017-02-22 | 铜陵市启动电子制造有限责任公司 | Supercapacitor electrode material added with manganese cobalt oxide foamed nickel composite material |
-
2018
- 2018-04-04 CN CN201810328399.4A patent/CN108485198A/en not_active Withdrawn
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101037225A (en) * | 2007-02-06 | 2007-09-19 | 南京航空航天大学 | Titanium dioxide nano thread, belt and tube block array and preparation method thereof |
| CN101659805A (en) * | 2009-09-24 | 2010-03-03 | 同济大学 | Preparation method of composite wave absorbing powder with wide frequency band |
| CN104370285A (en) * | 2014-10-23 | 2015-02-25 | 北京大学 | Method for macroscopically preparing high-quality graphene by using bio-mineralized material |
| CN105086448A (en) * | 2015-08-31 | 2015-11-25 | 苏州凯欧曼新材料科技有限公司 | High-dielectric constant composite material |
| CN105172297A (en) * | 2015-09-02 | 2015-12-23 | 苏州益可泰电子材料有限公司 | Flame-resistant and heat-resistant copper clad laminate preparation method |
| CN106449145A (en) * | 2016-11-08 | 2017-02-22 | 铜陵市启动电子制造有限责任公司 | Supercapacitor electrode material added with manganese cobalt oxide foamed nickel composite material |
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