CN106565919A - Low-cost polymer-encapsulated dielectric material and preparation method thereof - Google Patents
Low-cost polymer-encapsulated dielectric material and preparation method thereof Download PDFInfo
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- CN106565919A CN106565919A CN201610945939.4A CN201610945939A CN106565919A CN 106565919 A CN106565919 A CN 106565919A CN 201610945939 A CN201610945939 A CN 201610945939A CN 106565919 A CN106565919 A CN 106565919A
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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
- C08F292/00—Macromolecular compounds obtained by polymerising monomers on to inorganic materials
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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
- C08L51/00—Compositions of graft polymers in which the grafted component is obtained by reactions only involving carbon-to-carbon unsaturated bonds; Compositions of derivatives of such polymers
- C08L51/10—Compositions of graft polymers in which the grafted component is obtained by reactions only involving carbon-to-carbon unsaturated bonds; Compositions of derivatives of such polymers grafted on to inorganic materials
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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
Abstract
The invention discloses a low-cost polymer-encapsulated dielectric material which comprises the following raw materials in parts by weight: 0.4-1 part of zinc stearate, 2-3 parts of montan wax, 0.4-1 part of polyaspartic acid, 2-3 parts of allyl alcohol, 4-6 parts of a silane coupling agent kh550, 0.8-1.2 parts of trimethylamine, 0.2-0.3 part of 2-bromoisobutyryl bromide, 0.1-0.3 part of cuprous bromide, 71-80 parts of methyl methacrylate, 0.5-1 part of N,N,N',N",N"-pentamethyl diethylenetriamine, 1-2 parts of allylthiourea, 3-4 parts of tributyl citrate, 0.1-0.3 part of zinc naphthenate, 0.3-1 part of monoethanolamine, 31-40 parts of barium titanate and 0.3-1 part of hexamethyl cyclotrisiloxane. According to the low-cost polymer-encapsulated dielectric material disclosed by the invention, the montan wax and other raw materials are adopted; the energy consumption can be effectively lowered; and the environmental pollution can be reduced.
Description
Technical field
The present invention relates to dielectric material technical field, more particularly to a kind of inexpensive polymer overmold dielectric material and its system
Preparation Method.
Background technology
With the fast development of electric industry in recent years, requirement more and more higher of the people to high-dielectric composite material.
A following trend of electronic product is miniaturization：While improving performance, device do it is less and less.Electronic product is little
One of bottleneck of type is the volume of printed circuit board (PCB), because there is substantial amounts of passive element on circuit board, such as capacitor is occupied
Substantial amounts of space.Embedded printed circuit board is one of the effective ways for solving circuit board volume, and it is critical only that exploitation
High-dielectric composite material with superior function.Another purposes of high-dielectric composite material is electric stress control.Electrical equipment is big
Typeization with raising efficiency, but also can cause the electric stress in equipment suffered by material to increase, and be easily damaged.It would therefore be desirable to
The electric stress that new high-dielectric composite material is developed to meet large electric equipment controls requirement, promotes sending out for electric utility
Exhibition.Additionally, high-dielectric composite material can also be used to prepare high energy storage device to tackle demand of the current social to the energy.With
Energy storage device prepared by high-dielectric composite material has very high power density, in Aero-Space, sophisticated weapons and electric automobile
Aspect has critically important application potential.
The barium phthalate base polymer composites of present invention research are one of most potential high-dielectric composite materials, exploitation
This kind of high dielectric material with excellent properties has very to accelerating the development of Chinese national economy, lifting national security defence
Important meaning；
Data shows that adding nano-particle in polymer can increase the electrical conductivity of composite, increase leakage current.Inorganic
When filler is introduced in polymer, because between the two surface energy differs greatly, interaction force is weaker so that near interface is polymerized
The property of thing changes, such as the density of polymer chain reduces, and free volume becomes big, and vitrification point is reduced, and this can be caused
Electric charge is easily migrated.On the other hand, because the electrical property comparison in difference of inorganic particle and polymer is big, under the electric field, electric charge
Easily in interface aggregation, the charge density at this is significantly increased, can also increase the electrical conductivity at this.So, it is believed that,
In polymer composites, the boundary layer between inorganic filler and polymer is one semiconductor layer, big in composite
Partial charge is migrated by boundary layer.Therefore, we will reduce the leakage current of given composite, can be by changing
Interfacial structure is realizing.Such as, we can strengthen the interface interaction power between nano-particle and polymer, so as to increase interface
The density of neighbouring polymer chain, reduces free volume, improves vitrification point, suppresses charge migration to migrate in interface；
In the present invention, we are gathered using the atom transferred free radical of Barium metatitanate. surface in situ Methyl Methacrylate monomer
Close, PMMA polymer chains are directly connected to Barium metatitanate. surface in the way of covalent bond.Wherein ATRP be prepare it is nano combined
A kind of maturation method of material, with preferable feasibility and controllability.In the nano composite material for preparing in this way, often
One macromolecular chain is all connected on Nanosurface so that the polymer chain density of nano grain surface is significantly increased, and free volume subtracts
It is little, it is unfavorable for that electric charge is migrated in nano grain surface, such that it is able to reduce leakage current, reduce loss.Meanwhile, this method system
In standby composite, each nano-particle by polymer overmold, forms nucleocapsid structure, well dispersed, is difficult to each other
Directly contact, is also beneficial to reduce leakage current, and reduce loss lifts dielectric properties.
The content of the invention
The object of the invention is exactly to make up the defect of prior art, there is provided a kind of inexpensive polymer overmold dielectric material
And preparation method thereof.
The present invention is achieved by the following technical solutions：
A kind of inexpensive polymer overmold dielectric material, it is made up of the raw material of following weight parts：
Zinc stearate 0.4-1, lignite wax 2-3, poly-aspartate 0.4-1, propenyl 2-3, silane coupler kh5504-6, three second
Amine 0.8-1,2- bromine isobutyl acylbromide 0.2-0.3, cuprous bromide 0.1-0.3, methyl methacrylate 71-80, N, N, N ', N ", N "-
The support triamine 0.5-1 of pentamethyl second two, allylthiourea 1-2, tributyl citrate 3-4, zinc naphthenate 0.1-0.3, monoethanolamine
0.3-1, Barium metatitanate. 31-40, hexamethyl cyclotrisiloxane 0.3-1.
A kind of preparation method of described inexpensive polymer overmold dielectric material, comprises the following steps：
（1）Above-mentioned Barium metatitanate. is taken, in being added to the hydrogen peroxide solution that concentration is 25-30%, ultrasonic 10-20 minutes, 100- is sent into
In 105 DEG C of oil bath, insulated and stirred 3-4 hour, centrifugation is vacuum dried 10-12 hours at being deposited in 80-85 DEG C, obtain
Hydroxylating Barium metatitanate.；
（2）Above-mentioned poly-aspartate is taken, in being added to the dehydrated alcohol of its weight 106-130 times, is stirred, send into 87-90
DEG C water bath with thermostatic control in, add lignite wax, insulated and stirred 1-2 hour, discharging to add above-mentioned zinc naphthenate, stir to room temperature, obtain
Pre- mixed alcoholic liquid；
（3）Above-mentioned hydroxylating Barium metatitanate. is added in pre- mixed alcoholic liquid, ultrasonic 6-10 minutes, adds above-mentioned silane coupler
Kh550, is passed through nitrogen, the insulated and stirred 20-25 hour at 76-80 DEG C, centrifugation, and vacuum is done at being deposited in 80-85 DEG C
Dry 10-12 hours, obtain amination Barium metatitanate.；
（4）Above-mentioned amination Barium metatitanate., zinc stearate are mixed, in being added to the dichloromethane of compound weight 5-7 times, ultrasound
3-5 minutes, above-mentioned triethylamine is added, the standing and reacting 30-40 minute in ice-water bath, is slowly added dropwise above-mentioned 2- bromine isobutyl acylbromides,
Stirring reaction 3-4 hour after completion of dropping, discharging, the insulated and stirred 20-24 hour at 16-25 DEG C, centrifugation is normal by precipitation
Temperature is dried, and obtains bromination Barium metatitanate.；
（5）Above-mentioned allylthiourea is added in the dehydrated alcohol of its weight 20-30 times, it is 76-80 DEG C to rise high-temperature, insulation
Stirring 4-7 minutes, above-mentioned bromination Barium metatitanate., hexamethyl cyclotrisiloxane are added, ultrasonic 20-30 minutes, filtered, will be deposited in
10-12 hours are vacuum dried at 80-85 DEG C, modified bromination Barium metatitanate. is obtained；
（6）Above-mentioned modified bromination Barium metatitanate. is added in the dimethylformamide of its weight 30-40 times, ultrasonic 17-20 minutes,
Above-mentioned cuprous bromide, methyl methacrylate are added, nitrogen is passed through, above-mentioned N, N, N ', N is added ", the N " supports of-pentamethyl second two three
Amine, the insulated and stirred 20-25 hour at 60-65 DEG C, centrifugation is vacuum dried 10-14 hours at being deposited in 76-80 DEG C,
Compressing at 176-180 DEG C, pressure is in 20-30MPa.
It is an advantage of the invention that：The present invention aoxidizes barium titanate nano particle with strong oxidizer hydrogen peroxide solution first, increases
The number of Barium metatitanate. surface-active functional group-OH, promotes ensuing organic reagent to be modified, then with the ethoxy of γ-aminopropyl three
Base silane reacts, and forms amidized Barium metatitanate., introduces organo-functional group amino, and using Barium metatitanate. surface in situ methyl is caused
The atom transfer radical polymerization of methacrylate monomer, PMMA polymer chains titanium is directly connected in the way of covalent bond
Sour barium surface, the method for the present invention causes the polymer chain density of nano grain surface to be significantly increased, and free volume reduces, unfavorable
Migrate in nano grain surface in electric charge, such that it is able to reduce leakage current, reduce loss.Meanwhile, this method prepares compound
In material, each nano-particle by polymer overmold, forms nucleocapsid structure, well dispersed, is difficult to directly connect each other
Touch, be also beneficial to reduce leakage current, reduce loss lifts dielectric properties.The present invention, can be effective using raw materials such as lignite waxes
Energy saving, reduce environmental pollution.
Specific embodiment
A kind of inexpensive polymer overmold dielectric material, it is made up of the raw material of following weight parts：
Zinc stearate 0.4, lignite wax 2, poly-aspartate 0.4, propenyl 2, silane coupler kh5504, triethylamine 0.8,2 bromines
Isobutyl acylbromide 0.2, cuprous bromide 0.1, methyl methacrylate 71, N, N, N ', N ", N " pentamethyl second two supports triamine 0.5, allyl
Base thiourea 1, tributyl citrate 3, zinc naphthenate 0.1, monoethanolamine 0.3, Barium metatitanate. 31, hexamethyl cyclotrisiloxane 0.3.
A kind of preparation method of described inexpensive polymer overmold dielectric material, comprises the following steps：
（1）Above-mentioned Barium metatitanate. is taken, in being added to the hydrogen peroxide solution that concentration is 25%, ultrasound 10 minutes sends into 100 DEG C of oil bath
In, insulated and stirred 3 hours, centrifugation is vacuum dried 10 hours at being deposited in 80 DEG C, obtains hydroxylating Barium metatitanate.；
（2）Above-mentioned poly-aspartate is taken, in being added to the dehydrated alcohol of 106 times of its weight, is stirred, send into 87 DEG C of constant temperature
In water-bath, add lignite wax, insulated and stirred 1 hour, discharging to add above-mentioned zinc naphthenate, stir to room temperature, obtain pre- mixed alcoholic liquid；
（3）Above-mentioned hydroxylating Barium metatitanate. is added in pre- mixed alcoholic liquid, ultrasound 6 minutes adds above-mentioned silane coupler kh550,
Nitrogen is passed through, insulated and stirred 20 hours at 76 DEG C, centrifugation is vacuum dried 10 hours at being deposited in 80 DEG C, obtains amino
Change Barium metatitanate.；
（4）Above-mentioned amination Barium metatitanate., zinc stearate are mixed, in being added to the dichloromethane of 5 times of compound weight, ultrasound 3
Minute, above-mentioned triethylamine is added, standing and reacting 30 minutes in ice-water bath are slowly added dropwise above-mentioned 2 bromine isobutyl acylbromide, completion of dropping
Afterwards stirring reaction 3 hours, discharge, and insulated and stirred 20 hours at 16 DEG C, centrifugation will precipitate normal temperature drying, obtain titanium bromide
Sour barium；
（5）Above-mentioned allylthiourea is added in the dehydrated alcohol of 20 times of its weight, it is 76 DEG C to rise high-temperature, insulated and stirred 4
Minute, add above-mentioned bromination Barium metatitanate., hexamethyl cyclotrisiloxane, ultrasound 20 minutes to filter, vacuum is done at being deposited in 80 DEG C
Dry 10 hours, obtain modified bromination Barium metatitanate.；
（6）Above-mentioned modified bromination Barium metatitanate. is added in the dimethylformamide of 30 times of its weight, ultrasound 17 minutes, in addition
Cuprous bromide, methyl methacrylate are stated, nitrogen is passed through, above-mentioned N, N, N ', N is added ", " pentamethyl second two supports triamine to N, 60
Insulated and stirred 20 hours at DEG C, centrifugation is vacuum dried 10 hours at being deposited in 76 DEG C, compressing at 176 DEG C, pressure
Power is in 20MPa.
The dielectric constant of composite of the present invention is 1451.3 in 1 kHz.
Claims (2)
1. a kind of inexpensive polymer overmold dielectric material, it is characterised in that it is made up of the raw material of following weight parts：
Zinc stearate 0.4-1, lignite wax 2-3, poly-aspartate 0.4-1, propenyl 2-3, silane coupler kh5504-6, three second
Amine 0.8-1,2- bromine isobutyl acylbromide 0.2-0.3, cuprous bromide 0.1-0.3, methyl methacrylate 71-80, N, N, N ', N ", N "-
The support triamine 0.5-1 of pentamethyl second two, allylthiourea 1-2, tributyl citrate 3-4, zinc naphthenate 0.1-0.3, monoethanolamine
0.3-1, Barium metatitanate. 31-40, hexamethyl cyclotrisiloxane 0.3-1.
2. a kind of preparation method of inexpensive polymer overmold dielectric material as claimed in claim 1, it is characterised in that include
Following steps：
（1）Above-mentioned Barium metatitanate. is taken, in being added to the hydrogen peroxide solution that concentration is 25-30%, ultrasonic 10-20 minutes, 100- is sent into
In 105 DEG C of oil bath, insulated and stirred 3-4 hour, centrifugation is vacuum dried 10-12 hours at being deposited in 80-85 DEG C, obtain
Hydroxylating Barium metatitanate.；
（2）Above-mentioned poly-aspartate is taken, in being added to the dehydrated alcohol of its weight 106-130 times, is stirred, send into 87-90
DEG C water bath with thermostatic control in, add lignite wax, insulated and stirred 1-2 hour, discharging to add above-mentioned zinc naphthenate, stir to room temperature, obtain
Pre- mixed alcoholic liquid；
（3）Above-mentioned hydroxylating Barium metatitanate. is added in pre- mixed alcoholic liquid, ultrasonic 6-10 minutes, adds above-mentioned silane coupler
Kh550, is passed through nitrogen, the insulated and stirred 20-25 hour at 76-80 DEG C, centrifugation, and vacuum is done at being deposited in 80-85 DEG C
Dry 10-12 hours, obtain amination Barium metatitanate.；
（4）Above-mentioned amination Barium metatitanate., zinc stearate are mixed, in being added to the dichloromethane of compound weight 5-7 times, ultrasound
3-5 minutes, above-mentioned triethylamine is added, the standing and reacting 30-40 minute in ice-water bath, is slowly added dropwise above-mentioned 2- bromine isobutyl acylbromides,
Stirring reaction 3-4 hour after completion of dropping, discharging, the insulated and stirred 20-24 hour at 16-25 DEG C, centrifugation is normal by precipitation
Temperature is dried, and obtains bromination Barium metatitanate.；
（5）Above-mentioned allylthiourea is added in the dehydrated alcohol of its weight 20-30 times, it is 76-80 DEG C to rise high-temperature, insulation
Stirring 4-7 minutes, above-mentioned bromination Barium metatitanate., hexamethyl cyclotrisiloxane are added, ultrasonic 20-30 minutes, filtered, will be deposited in
10-12 hours are vacuum dried at 80-85 DEG C, modified bromination Barium metatitanate. is obtained；
（6）Above-mentioned modified bromination Barium metatitanate. is added in the dimethylformamide of its weight 30-40 times, ultrasonic 17-20 minutes,
Above-mentioned cuprous bromide, methyl methacrylate are added, nitrogen is passed through, above-mentioned N, N, N ', N is added ", the N " supports of-pentamethyl second two three
Amine, the insulated and stirred 20-25 hour at 60-65 DEG C, centrifugation is vacuum dried 10-14 hours at being deposited in 76-80 DEG C,
Compressing at 176-180 DEG C, pressure is in 20-30MPa.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201610945939.4A CN106565919A (en) | 2016-10-26 | 2016-10-26 | Low-cost polymer-encapsulated dielectric material and preparation method thereof |
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| CN201610945939.4A CN106565919A (en) | 2016-10-26 | 2016-10-26 | Low-cost polymer-encapsulated dielectric material and preparation method thereof |
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| CN106565919A true CN106565919A (en) | 2017-04-19 |
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