CN106565920A - Nylon composite polymer-coated dielectric material and preparation method thereof - Google Patents
Nylon composite polymer-coated dielectric material and preparation method thereof Download PDFInfo
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- CN106565920A CN106565920A CN201610962725.8A CN201610962725A CN106565920A CN 106565920 A CN106565920 A CN 106565920A CN 201610962725 A CN201610962725 A CN 201610962725A CN 106565920 A CN106565920 A CN 106565920A
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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
- C08L2201/00—Properties
- C08L2201/08—Stabilised against heat, light or radiation or oxydation
Abstract
The invention discloses a nylon composite polymer-coated dielectric material. The nylon composite polymer-coated dielectric material is composed of the following raw materials in parts by weight: 71-80 parts of methyl methacrylate, 10-14 parts of nylon PA66, 0.8-2 parts of triethanolamine borate, 31-40 parts of barium titanate, 4-6 parts of silane coupling agent kh550, 0.8-1 part of triethylamine, 0.2-0.3 part of 2-bromoisobutyryl bromide, 0.1-0.3 part of cuprous bromide, 0.4-1 part of N,N,N',N'',N''-pentamethyldiethylenetriamine, 0.3-1 part of tetrabutylammonium bromide, 0.4-1 part of zinc stearate, 2-4 parts of terpilenol, 0.1-0.2 part of cerium oxide, 0.7-1 part of fatty acyl diethanol amine and 0.5-1 part of ethylene thiourea. According to the nylon composite polymer-coated dielectric material disclosed by the invention, the added nylon PA66 is capable of effectively increasing the surface hardness and strength of the finished composite material, improving the hydrophobicity thereof, and improving the weather resistance and stability thereof.
Description
Technical field
The present invention relates to dielectric material technical field, more particularly to a kind of nylon composition polymer cladding dielectric material and its
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 titanate surface in situ Methyl Methacrylate monomer
Close, PMMA polymer chains are directly connected to barium titanate 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 nylon composition polymer coats dielectric material
Material and preparation method thereof.
The present invention is achieved by the following technical solutions：
A kind of nylon composition polymer coats dielectric material, and it is made up of the raw material of following weight parts：
Methyl methacrylate 71-80, nylon PA6610-14, triethanolamine borate 0.8-2, barium titanate 31-40, silane idol
Connection agent kh5504-6, triethylamine 0.8-1,2- bromine isobutyl acylbromide 0.2-0.3, cuprous bromide 0.1-0.3, N, N, N ', N ", N "-five
Methyl second two support triamine 0.4-1, TBAB 0.3-1, zinc stearate 0.4-1, terpinol 2-4, cerium oxide 0.1-0.2,
Fatty diglycollic amide 0.7-1, ethylene thiourea 0.5-1.
A kind of described nylon composition polymer coats the preparation method of dielectric material, comprises the following steps：
（1）Above-mentioned fatty diglycollic amide is added in the deionized water of its weight 27-30 times, is stirred, in addition
Cerium oxide is stated, ultrasonic 3-4 minutes, acid amides dispersion liquid is obtained；
（2）Above-mentioned barium titanate is taken, in being added to the hydrogen peroxide solution that concentration is 25-30%, above-mentioned acid amides dispersion liquid, ultrasound is added
10-20 minutes, in sending into 100-105 DEG C of oil bath, insulated and stirred 3-4 hour, centrifugation is true at being deposited in 80-85 DEG C
Sky is dried 10-12 hours, obtains hydroxylating barium titanate；
（3）Above-mentioned hydroxylating barium titanate is added in absolute ethyl alcohol, 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, adds above-mentioned terpinol, stirs to normal temperature, centrifugation point
From, 10-12 hours are vacuum dried at 80-85 DEG C will be deposited in, obtain amination barium titanate；
（4）Above-mentioned nylon PA66 is added in the dimethylformamide of its weight 4-7 times, it is 87-90 DEG C to rise high-temperature, insulation
Stirring 13-20 minutes, above-mentioned zinc stearate is added, stirred to normal temperature, mixed with above-mentioned amination barium titanate, stirred, mistake
Filter, precipitation dimethylformamide, deionized water are washed 3-4 time successively, and 1-2 hours are vacuum dried at 50-60 DEG C, obtain Buddhist nun
Imperial composite titanic acid barium；
（5）Above-mentioned nylon composite titanic acid barium is added in the dichloromethane of its weight 5-7 times, ultrasonic 3-5 minutes, is added above-mentioned
Triethylamine, stands reaction 30-40 minutes in ice-water bath, is slowly added dropwise above-mentioned 2- bromine isobutyl acylbromides, stirs anti-after completion of dropping
3-4 hours are answered, is discharged, the insulated and stirred 20-24 hour at 16-25 DEG C, centrifugation, vacuum is done at being deposited in 80-85 DEG C
Dry 10-12 hours, obtain bromination barium titanate；
（6）Above-mentioned bromination barium titanate is added in the dimethylformamide of its weight 30-40 times, ultrasonic 17-20 minutes, is added
Above-mentioned cuprous bromide, methyl methacrylate, are passed through nitrogen, add remaining each raw material, insulated and stirred 20-25 at 60-65 DEG C
Hour, 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 titanate 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 titanate, introduces organo-functional group amino, and using barium titanate surface in situ methyl is caused
The ATRP 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 nylon PA66 that the present invention is added, can be effective
Case hardness, intensity and the hydrophobicity of finished composite material are improved, the weatherability and stability of finished product is improved.
Specific embodiment
A kind of nylon composition polymer coats dielectric material, and it is made up of the raw material of following weight parts：
Methyl methacrylate 71, nylon PA6610, triethanolamine borate 0.8, barium titanate 31, silane coupler kh5504,
Triethylamine 0.8,2 bromine isobutyl acylbromides 0.2, cuprous bromide 0.1, N, N, N ', N ", N " pentamethyl second two support triamine 0.4, tetrabutyl bromine
Change ammonium 0.3, zinc stearate 0.4, terpinol 2, cerium oxide 0.1, fatty diglycollic amide 0.7, ethylene thiourea 0.5.
A kind of described nylon composition polymer coats the preparation method of dielectric material, comprises the following steps：
（1）Above-mentioned fatty diglycollic amide is added in the deionized water of 27 times of its weight, is stirred, add above-mentioned oxygen
Change cerium, ultrasound 3 minutes obtains acid amides dispersion liquid；
（2）Above-mentioned barium titanate is taken, in being added to the hydrogen peroxide solution that concentration is 25%, above-mentioned acid amides dispersion liquid, 10 points of ultrasound is added
Clock, in sending into 100 DEG C of oil bath, insulated and stirred 3 hours, centrifugation is vacuum dried 10 hours at being deposited in 80 DEG C, obtains hydroxyl
Base barium titanate；
（3）Above-mentioned hydroxylating barium titanate is added in absolute ethyl alcohol, ultrasound 6 minutes adds above-mentioned silane coupler kh550,
Nitrogen is passed through, insulated and stirred 20 hours at 76 DEG C add above-mentioned terpinol, stir to normal temperature, centrifugation, will be deposited in 80
It is vacuum dried 10 hours at DEG C, obtains amination barium titanate；
（4）Above-mentioned nylon PA66 is added in the dimethylformamide of 4 times of its weight, it is 87 DEG C to rise high-temperature, insulated and stirred
13 minutes, above-mentioned zinc stearate is added, stirred to normal temperature, mixed with above-mentioned amination barium titanate, stirred, filtered, will be heavy
Shallow lake dimethylformamide, deionized water are washed successively 3 times, are vacuum dried 1 hour at 50 DEG C, obtain nylon composite titanic acid barium；
（5）Above-mentioned nylon composite titanic acid barium is added in the dichloromethane of 5 times of its weight, ultrasound 3 minutes adds above-mentioned three second
Amine, stands reaction 30 minutes in ice-water bath, is slowly added dropwise above-mentioned 2 bromine isobutyl acylbromide, stirring reaction 3 hours after completion of dropping,
Discharging, insulated and stirred 20 hours at 16 DEG C, centrifugation is vacuum dried 10 hours at being deposited in 80 DEG C, obtains bromination metatitanic acid
Barium；
（6）Above-mentioned bromination barium titanate is added in the dimethylformamide of 30 times of its weight, ultrasound 17 minutes adds above-mentioned bromine
Change cuprous, methyl methacrylate, be passed through nitrogen, add remaining each raw material, insulated and stirred 20 hours at 60 DEG C, centrifugation point
From, it is vacuum dried 10 hours at 76 DEG C will be deposited in, compressing at 176 DEG C, pressure is in 20MPa.
The dielectric constant of composite of the present invention is 1452.4 in 1 kHz.
Claims (2)
1. a kind of nylon composition polymer coats dielectric material, it is characterised in that it is made up of the raw material of following weight parts：
Methyl methacrylate 71-80, nylon PA6610-14, triethanolamine borate 0.8-2, barium titanate 31-40, silane idol
Connection agent kh5504-6, triethylamine 0.8-1,2- bromine isobutyl acylbromide 0.2-0.3, cuprous bromide 0.1-0.3, N, N, N ', N ", N "-five
Methyl second two support triamine 0.4-1, TBAB 0.3-1, zinc stearate 0.4-1, terpinol 2-4, cerium oxide 0.1-0.2,
Fatty diglycollic amide 0.7-1, ethylene thiourea 0.5-1.
2. a kind of nylon composition polymer as claimed in claim 1 coats the preparation method of dielectric material, it is characterised in that bag
Include following steps：
（1）Above-mentioned fatty diglycollic amide is added in the deionized water of its weight 27-30 times, is stirred, in addition
Cerium oxide is stated, ultrasonic 3-4 minutes, acid amides dispersion liquid is obtained；
（2）Above-mentioned barium titanate is taken, in being added to the hydrogen peroxide solution that concentration is 25-30%, above-mentioned acid amides dispersion liquid, ultrasound is added
10-20 minutes, in sending into 100-105 DEG C of oil bath, insulated and stirred 3-4 hour, centrifugation is true at being deposited in 80-85 DEG C
Sky is dried 10-12 hours, obtains hydroxylating barium titanate；
（3）Above-mentioned hydroxylating barium titanate is added in absolute ethyl alcohol, 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, adds above-mentioned terpinol, stirs to normal temperature, centrifugation point
From, 10-12 hours are vacuum dried at 80-85 DEG C will be deposited in, obtain amination barium titanate；
（4）Above-mentioned nylon PA66 is added in the dimethylformamide of its weight 4-7 times, it is 87-90 DEG C to rise high-temperature, insulation
Stirring 13-20 minutes, above-mentioned zinc stearate is added, stirred to normal temperature, mixed with above-mentioned amination barium titanate, stirred, mistake
Filter, precipitation dimethylformamide, deionized water are washed 3-4 time successively, and 1-2 hours are vacuum dried at 50-60 DEG C, obtain Buddhist nun
Imperial composite titanic acid barium；
（5）Above-mentioned nylon composite titanic acid barium is added in the dichloromethane of its weight 5-7 times, ultrasonic 3-5 minutes, is added above-mentioned
Triethylamine, stands reaction 30-40 minutes in ice-water bath, is slowly added dropwise above-mentioned 2- bromine isobutyl acylbromides, stirs anti-after completion of dropping
3-4 hours are answered, is discharged, the insulated and stirred 20-24 hour at 16-25 DEG C, centrifugation, vacuum is done at being deposited in 80-85 DEG C
Dry 10-12 hours, obtain bromination barium titanate；
（6）Above-mentioned bromination barium titanate is added in the dimethylformamide of its weight 30-40 times, ultrasonic 17-20 minutes, is added
Above-mentioned cuprous bromide, methyl methacrylate, are passed through nitrogen, add remaining each raw material, insulated and stirred 20-25 at 60-65 DEG C
Hour, 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.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610962725.8A CN106565920A (en) | 2016-10-26 | 2016-10-26 | Nylon composite polymer-coated dielectric material and preparation method thereof |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610962725.8A CN106565920A (en) | 2016-10-26 | 2016-10-26 | Nylon composite polymer-coated dielectric material and preparation method thereof |
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| CN106565920A true CN106565920A (en) | 2017-04-19 |
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| CN201610962725.8A Withdrawn CN106565920A (en) | 2016-10-26 | 2016-10-26 | Nylon composite polymer-coated dielectric material and preparation method thereof |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113444288A (en) * | 2021-06-10 | 2021-09-28 | 南昌工程学院 | Dioxaborane group modified barium titanate with reversible crosslinking structure and preparation method thereof |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105367811A (en) * | 2015-10-28 | 2016-03-02 | 清华大学 | Carbonyl-containing material-coated barium titanate/polymer composite film and preparation method thereof and application |
| CN105623092A (en) * | 2016-02-03 | 2016-06-01 | 安徽紫金新材料科技股份有限公司 | Polypropylene-nylon composite plastic thin film and preparation method thereof |
| CN105885402A (en) * | 2016-04-29 | 2016-08-24 | 安徽安缆模具有限公司 | Wear-resistant nylon mold material and preparation method thereof |
-
2016
- 2016-10-26 CN CN201610962725.8A patent/CN106565920A/en not_active Withdrawn
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105367811A (en) * | 2015-10-28 | 2016-03-02 | 清华大学 | Carbonyl-containing material-coated barium titanate/polymer composite film and preparation method thereof and application |
| CN105623092A (en) * | 2016-02-03 | 2016-06-01 | 安徽紫金新材料科技股份有限公司 | Polypropylene-nylon composite plastic thin film and preparation method thereof |
| CN105885402A (en) * | 2016-04-29 | 2016-08-24 | 安徽安缆模具有限公司 | Wear-resistant nylon mold material and preparation method thereof |
Non-Patent Citations (1)
| Title |
|---|
| LIYUAN XIE, ETC: "Core-shell structured poly(methyl methacrylate)/BaTiO3 nanocomposites prepared by in situ atom transfer radical polymerization: a route to high dielectric constant materials with the inherent low loss of the base polymer", 《JOURNAL OF MATERIAL CHEMISTRY》 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113444288A (en) * | 2021-06-10 | 2021-09-28 | 南昌工程学院 | Dioxaborane group modified barium titanate with reversible crosslinking structure and preparation method thereof |
| CN113444288B (en) * | 2021-06-10 | 2022-06-07 | 南昌工程学院 | Dioxaborane group modified barium titanate with reversible crosslinking structure and preparation method thereof |
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