CN106565917A - Diatomite modified polymer coated dielectric material and preparation method thereof - Google Patents
Diatomite modified polymer coated dielectric material and preparation method thereof Download PDFInfo
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- CN106565917A CN106565917A CN201610945914.4A CN201610945914A CN106565917A CN 106565917 A CN106565917 A CN 106565917A CN 201610945914 A CN201610945914 A CN 201610945914A CN 106565917 A CN106565917 A CN 106565917A
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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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- 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
- C08K13/00—Use of mixtures of ingredients not covered by one single of the preceding main groups, each of these compounds being essential
- C08K13/06—Pretreated ingredients and ingredients covered by the main groups C08K3/00 - C08K7/00
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
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- 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
- C08K7/00—Use of ingredients characterised by shape
- C08K7/22—Expanded, porous or hollow particles
- C08K7/24—Expanded, porous or hollow particles inorganic
- C08K7/26—Silicon- containing compounds
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L1/00—Compositions of cellulose, modified cellulose or cellulose derivatives
- C08L1/08—Cellulose derivatives
- C08L1/16—Esters of inorganic acids
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
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- 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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Abstract
The invention discloses a diatomite modified polymer coated dielectric material. The diatomite modified polymer coated dielectric material is composed of, by weight, 0.7-1 part of ammonium ethoxylated alkyl sulfate, 1-2 parts of phosphorylated cellulose, 0.1-0.3 part of ricinoleic acid, 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-bromopropionyl bromide, 0.1-0.3 part of cuprous bromide, 71-80 parts of methyl methacrylate, 0.4-1 part of N, N, N', N'', N''-pentamethyl diethylenetriamine, 5-7 parts of diatomite, 1-2 parts of aluminum dihydrogen phosphate, 0.6-1 part of dialkyl hydroquinone, 2-3 parts of triisopropanolamine and 1-2 parts of oxidized graphene. Due to the fact that the diatomite is added into the diatomite modified polymer coated dielectric material, the surface hardness and resistance of the finished product can be effectively improved.
Description
Technical field
The present invention relates to dielectric material technical field, more particularly to a kind of diatomite modified polymer overmold 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 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 diatomite modified polymer overmold dielectric
Material and preparation method thereof.
The present invention is achieved by the following technical solutions：
A kind of diatomite modified polymer overmold dielectric material, it is made up of the raw material of following weight parts：
Ethoxylated alkyl ammonium sulfate 0.7-1, cellulose phosphate 1-2, castor oil acid 0.1-0.3, Barium metatitanate. 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, methyl methacrylate
The support triamine 0.4-1 of 71-80, N, N, N ', N ", N "-pentamethyls second two, kieselguhr 5-7, aluminium dihydrogen phosphate 1-2, dialkyl group are to hexichol
Phenol 0.6-1, triisopropanolamine 2-3, graphene oxide 1-2.
A kind of preparation method of described diatomite modified polymer overmold dielectric material, comprises the following steps：
（1）Above-mentioned cellulose phosphate is added in the deionized water of its weight 17-20 times, it is 60-70 DEG C to rise high-temperature, is added
Above-mentioned triisopropanolamine, insulated and stirred 5-9 minute, adds above-mentioned graphene oxide, stirs to room temperature, filters, by precipitation washing
2-3 time, 1-2 hours are vacuum dried at 47-50 DEG C, obtain fibre modification Graphene；
（2）Above-mentioned Barium metatitanate. is taken, is mixed with fibre modification Graphene, in being added to the hydrogen peroxide solution that concentration is 25-30%, plus
Enter above-mentioned ethoxylated alkyl ammonium sulfate, ultrasonic 10-20 minutes, in sending into 100-105 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.；
（3）Above-mentioned hydroxylating Barium metatitanate. is added in dehydrated 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, centrifugation, and vacuum is done at being deposited in 80-85 DEG C
Dry 10-12 hours, obtain amination Barium metatitanate.；
（4）Above-mentioned dialkyl group is added in the dehydrated alcohol of its weight 15-20 times to biphenol, it is 57-60 DEG C to rise high-temperature,
Insulated and stirred 10-13 minute, above-mentioned castor oil acid is added, stirred to room temperature, add above-mentioned kieselguhr, ultrasonic 3-4 minutes, mistake
Filter, by precipitation washing 2-3 time, is vacuum dried 1-2 hours at 40-50 DEG C, obtains modification infusorial earth；
（5）Above-mentioned amination Barium metatitanate., modification infusorial earth are mixed, in being added to the dichloromethane of compound weight 5-7 times, is surpassed
Sound 3-5 minutes, above-mentioned triethylamine is added, the standing and reacting 30-40 minute in ice-water bath, be slowly added dropwise above-mentioned 2- bromines isobutyryl
Bromine, stirring reaction 3-4 hour after completion of dropping, discharging, the insulated and stirred 20-24 hour at 16-25 DEG C, centrifugation will be heavy
Form sediment and 10-12 hours are vacuum dried at 80-85 DEG C, obtain bromination Barium metatitanate.；
（6）Above-mentioned bromination Barium metatitanate. 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 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.Present invention adds kieselguhr, can effectively carry
The case hardness and resistance of high finished product.
Specific embodiment
A kind of diatomite modified polymer overmold dielectric material, it is made up of the raw material of following weight parts：
Ethoxylated alkyl ammonium sulfate 0.7, cellulose phosphate 1, castor oil acid 0.1, Barium metatitanate. 31, silane coupler kh5504,
Triethylamine 0.8,2 bromine isobutyl acylbromides 0.2, cuprous bromide 0.1, methyl methacrylate 71, N, N, N ', N ", N " pentamethyl second two
Support triamine 0.4, kieselguhr 5, aluminium dihydrogen phosphate 1, dialkyl group are to biphenol 0.6, triisopropanolamine 2, graphene oxide 1.
A kind of preparation method of described diatomite modified polymer overmold dielectric material, comprises the following steps：
（1）Above-mentioned cellulose phosphate is added in the deionized water of 17 times of its weight, it is 60 DEG C to rise high-temperature, adds above-mentioned three
Isopropanolamine, insulated and stirred 5 minutes adds above-mentioned graphene oxide, stirs to room temperature, filters, by precipitation washing 2 times, 47
It is vacuum dried 1 hour at DEG C, obtains fibre modification Graphene；
（2）Above-mentioned Barium metatitanate. is taken, is mixed with fibre modification Graphene, in being added to the hydrogen peroxide solution that concentration is 25%, in addition
Ethoxylated alkyl ammonium sulfate is stated, it is ultrasonic 10 minutes, in sending into 100 DEG C of oil bath, insulated and stirred 3 hours, centrifugation will be heavy
Form sediment and be vacuum dried 10 hours at 80 DEG C, obtain hydroxylating Barium metatitanate.；
（3）Above-mentioned hydroxylating Barium metatitanate. is added in dehydrated alcohol, 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 dialkyl group is added in the dehydrated alcohol of 15 times of its weight to biphenol, it is 57 DEG C to rise high-temperature, and insulation is stirred
Mix 10 minutes, add above-mentioned castor oil acid, stir to room temperature, add above-mentioned kieselguhr, ultrasound 3 minutes to filter, by precipitation washing
2 times, it is vacuum dried 1 hour at 40 DEG C, obtains modification infusorial earth；
（5）Above-mentioned amination Barium metatitanate., modification infusorial earth are mixed, in being added to the dichloromethane of 5 times of compound weight, ultrasound
3 minutes, above-mentioned triethylamine is added, standing and reacting 30 minutes in ice-water bath are slowly added dropwise above-mentioned 2 bromine isobutyl acylbromide, drip
Stirring reaction 3 hours after finishing, discharging, insulated and stirred 20 hours at 16 DEG C, centrifugation is vacuum dried at being deposited in 80 DEG C
10 hours, obtain bromination Barium metatitanate.；
（6）Above-mentioned bromination Barium metatitanate. 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 1432.2 in 1 kHz.
Claims (2)
1. a kind of diatomite modified polymer overmold dielectric material, it is characterised in that it is made up of the raw material of following weight parts
's：
Ethoxylated alkyl ammonium sulfate 0.7-1, cellulose phosphate 1-2, castor oil acid 0.1-0.3, Barium metatitanate. 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, methyl methacrylate
The support triamine 0.4-1 of 71-80, N, N, N ', N ", N "-pentamethyls second two, kieselguhr 5-7, aluminium dihydrogen phosphate 1-2, dialkyl group are to hexichol
Phenol 0.6-1, triisopropanolamine 2-3, graphene oxide 1-2.
2. a kind of preparation method of diatomite modified polymer overmold dielectric material as claimed in claim 1, it is characterised in that
Comprise the following steps：
（1）Above-mentioned cellulose phosphate is added in the deionized water of its weight 17-20 times, it is 60-70 DEG C to rise high-temperature, is added
Above-mentioned triisopropanolamine, insulated and stirred 5-9 minute, adds above-mentioned graphene oxide, stirs to room temperature, filters, by precipitation washing
2-3 time, 1-2 hours are vacuum dried at 47-50 DEG C, obtain fibre modification Graphene；
（2）Above-mentioned Barium metatitanate. is taken, is mixed with fibre modification Graphene, in being added to the hydrogen peroxide solution that concentration is 25-30%, plus
Enter above-mentioned ethoxylated alkyl ammonium sulfate, ultrasonic 10-20 minutes, in sending into 100-105 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.；
（3）Above-mentioned hydroxylating Barium metatitanate. is added in dehydrated 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, centrifugation, and vacuum is done at being deposited in 80-85 DEG C
Dry 10-12 hours, obtain amination Barium metatitanate.；
（4）Above-mentioned dialkyl group is added in the dehydrated alcohol of its weight 15-20 times to biphenol, it is 57-60 DEG C to rise high-temperature,
Insulated and stirred 10-13 minute, above-mentioned castor oil acid is added, stirred to room temperature, add above-mentioned kieselguhr, ultrasonic 3-4 minutes, mistake
Filter, by precipitation washing 2-3 time, is vacuum dried 1-2 hours at 40-50 DEG C, obtains modification infusorial earth；
（5）Above-mentioned amination Barium metatitanate., modification infusorial earth are mixed, in being added to the dichloromethane of compound weight 5-7 times, is surpassed
Sound 3-5 minutes, above-mentioned triethylamine is added, the standing and reacting 30-40 minute in ice-water bath, be slowly added dropwise above-mentioned 2- bromines isobutyryl
Bromine, stirring reaction 3-4 hour after completion of dropping, discharging, the insulated and stirred 20-24 hour at 16-25 DEG C, centrifugation will be heavy
Form sediment and 10-12 hours are vacuum dried at 80-85 DEG C, obtain bromination Barium metatitanate.；
（6）Above-mentioned bromination Barium metatitanate. 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.
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| CN201610945914.4A CN106565917A (en) | 2016-10-26 | 2016-10-26 | Diatomite modified polymer coated dielectric material and preparation method thereof |
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102417363A (en) * | 2011-08-02 | 2012-04-18 | 中国科学院化学研究所 | Micron-nano-sized porous composite material and preparation method thereof |
| CN102827438A (en) * | 2012-09-20 | 2012-12-19 | 江苏上上电缆集团有限公司 | Cable filler composition |
| CN102875871A (en) * | 2012-09-20 | 2013-01-16 | 江苏上上电缆集团有限公司 | Cable filling material capable of improving transmission capacity of cable |
| CN104774296A (en) * | 2015-03-25 | 2015-07-15 | 天长市开林化工有限公司 | High-performance super-hydrophobic graphene modified fluorosilicone resin material and preparation method thereof |
| CN105985052A (en) * | 2016-01-15 | 2016-10-05 | 安徽鑫润新型材料有限公司 | Efficient polycarboxylic acid water reducing agent with additional modified celluloses |
-
2016
- 2016-10-26 CN CN201610945914.4A patent/CN106565917A/en not_active Withdrawn
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102417363A (en) * | 2011-08-02 | 2012-04-18 | 中国科学院化学研究所 | Micron-nano-sized porous composite material and preparation method thereof |
| CN102827438A (en) * | 2012-09-20 | 2012-12-19 | 江苏上上电缆集团有限公司 | Cable filler composition |
| CN102875871A (en) * | 2012-09-20 | 2013-01-16 | 江苏上上电缆集团有限公司 | Cable filling material capable of improving transmission capacity of cable |
| CN104774296A (en) * | 2015-03-25 | 2015-07-15 | 天长市开林化工有限公司 | High-performance super-hydrophobic graphene modified fluorosilicone resin material and preparation method thereof |
| CN105985052A (en) * | 2016-01-15 | 2016-10-05 | 安徽鑫润新型材料有限公司 | Efficient polycarboxylic acid water reducing agent with additional modified celluloses |
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》 * |
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