CN106566144A - Aluminium sol high-dielectric material and preparation method thereof - Google Patents
Aluminium sol high-dielectric material and preparation method thereof Download PDFInfo
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- CN106566144A CN106566144A CN201610908180.2A CN201610908180A CN106566144A CN 106566144 A CN106566144 A CN 106566144A CN 201610908180 A CN201610908180 A CN 201610908180A CN 106566144 A CN106566144 A CN 106566144A
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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
- C08L27/00—Compositions of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Compositions of derivatives of such polymers
- C08L27/02—Compositions of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Compositions of derivatives of such polymers not modified by chemical after-treatment
- C08L27/12—Compositions of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Compositions of derivatives of such polymers not modified by chemical after-treatment containing fluorine atoms
- C08L27/16—Homopolymers or copolymers or vinylidene fluoride
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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
- 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 an aluminium sol high-dielectric material. The material is prepared from raw materials in parts by weight as follows: 60-75 parts of barium titanate, 10-14 parts of gamma-aminopropyltriethoxysilane, 2.6-3 parts of 3,5-diaminobenzoic acid, 6-8 parts of triphenyl phosphite, 3-4 parts of pyridine, 0.02-0.03 parts of lithium chloride, 4.3-5 parts of cuprous bromide, 7-10 parts of polyvinylidene fluoride, 0.4-1 part of hexamethylphosphoramide, 4-5 parts of aluminium isopropoxide, 2-3 parts of dibutyl maleate, 0.2-0.5 parts of alkenyl succinic anhydride, 0.3-1 part of dibutyltin dilaurate, 3-4 parts of polyethylene glycol, 0.6-1 part of dialkyl hydroquinone and 2-4 parts of kieselguhr. The aluminium isopropoxide is used as a precursor, and the prepared aluminium sol can effectively improve the compatibility of materials and improve the surface resistance and the stability of a finished product.
Description
Technical field
The present invention relates to dielectric material technical field, more particularly to a kind of Alumina gel high dielectric material and preparation method thereof.
Background technology
High dielectric material has application widely, and it is dielectric constant to assess one of major parameter of the material property.
Therefore, high performance dielectric material is prepared, seeks to improve its dielectric constant first.The dielectric constant of dielectric substance is main
Stem from the polarization of material internal, want the dielectric constant for improving material, herein the intensity of necessary reinforcing material internal polarization.Electricity
The molecule mechanism that medium polarizes under the electric field is more complicated, main to include four kinds：Interfacial polarization, dipole orientation, ionic polarization and
Electronic polarization.Wherein, dipole orientation, ionic polarization and electronic polarization are relevant with the composition of material and their intrinsic electrical properties, and
Interfacial polarization is also relevant with the interfacial structure of composite except having outside the Pass with the intrinsic electrical property of material.In order to prepare with height
The nano-polymer composite material of dielectric constant, the present invention by select suitable high dielectric nano filler and polymeric matrix come
Improve dipole orientation, ionic polarization and electronic polarization, and the interfacial structure of uniqueness is designed by the distinctive structure of nanometer carrying
High interfacial polarization, so as to greatly improve the dielectric constant of composite；
First, the present invention selects nano barium titanate titanate particle as filler to improve the dielectric constant of polymer composites, nanometer
Barium titanate is a kind of common ferroelectric ceramics, can spontaneous polarization, have very high dielectric constant, meanwhile, barium titanate also has fine
Insulating properties and stability, its surface there are reactive hydroxyl groups functional group, be to design special interfacial structure below to carry
Feasibility is supplied.Common high dielectric filler with other, such as titanium dioxide, zinc oxide is compared with zirconium oxide inorganic particle, titanium
Sour barium has very big advantage, therefore is widely used in preparing high dielectric polymer composite.People also study discovery, select and receive
Rice filler from micron filler than being more beneficial for improving the electrical property of composite, on the one hand, Nano filling has larger ratio table
Area, can increase the interfacial area in composite, so as to strengthen interfacial polarization, improve dielectric constant；On the other hand, it is past poly-
Adding Nano filling in compound can improve the dielectric strength of composite, lift the practical value of material；
In addition, the present invention forms a kind of special core-shell structure copolymer knot also by coating barium titanate nano particle with ultrabranching polyamide
Structure, improves the dielectric constant of composite.The interfacial polarization of composite except having outside the Pass with the property of composite each component,
It is also relevant with the interfacial structure of composite.It is known that interfacial polarization is due to electric charge, and in interface, aggregation causes, because
This, the present invention can be by being designed with the special construction beneficial to accumulation to improve interfacial polarization.Here, present invention choosing
Barium titanate is coated with ultrabranching polyamide, is because being compared with other polymers, ultrabranching polyamide has higher electrical conductivity
And dielectric constant.One layer of ultrabranching polyamide is inserted in interface, electric charge can be promoted toward interface aggregates, so as to improve interface pole
Change.
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 Alumina gel high dielectric material and its preparation
Method.
The present invention is achieved by the following technical solutions：
A kind of Alumina gel high dielectric material, it is made up of the raw material of following weight parts：
Barium titanate 60-75, gamma-aminopropyl-triethoxy-silane 10-14,3,5- diaminobenzoic acid 2.6-3, triphenyl phosphite
6-8, pyridine 3-4, lithium chloride 0.02-0.03, cuprous bromide 4.3-5, Kynoar 7-10, HMPA 0.4-1,
Aluminium isopropoxide 4-5, dibutyl maleate 2-3, alkenyl succinic anhydride 0.2-0.5, dibutyl tin laurate 0.3-1, poly- second two
Alcohol 3-4, dialkyl group are to biphenol 0.6-1, diatomite 2-4.
A kind of preparation method of described Alumina gel high dielectric material, comprises the following steps：
（1）Above-mentioned aluminium isopropoxide is added in the deionized water of its weight 27-30 times, is stirred, liter high-temperature is 61-70
DEG C, insulated and stirred 10-15 minute, above-mentioned alkenyl succinic anhydride is added, continue insulated and stirred 30-40 minute, 5-7mol/l is added dropwise
NaOH, regulation pH is 11-13, and the slow temperature that reduces is 36-40 DEG C, insulated and stirred 18-20 minute, adds above-mentioned pregnancy
Base phosphoric triamide, stirs to normal temperature, in being sent to baking oven, is dried completely at 85-90 DEG C, obtains modified Alumina gel；
（2）Above-mentioned barium titanate 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 titanate；
（3）Above-mentioned dialkyl group is added in the absolute ethyl alcohol of its weight 37-40 times to biphenol, is stirred, rise high-temperature
For 60-64 DEG C, insulated and stirred 10-14 minute, above-mentioned modified Alumina gel is added, ultrasonic 3-4 minutes, obtain colloidal sol alcohol liquid；
（4）Above-mentioned hydroxylating barium titanate is added in absolute ethyl alcohol, ultrasonic 6-10 minutes, adds the above-mentioned second of γ-aminopropyl three
TMOS, is passed through nitrogen, the insulated and stirred 20-25 hour at 76-80 DEG C, adds above-mentioned colloidal sol alcohol liquid, stirs, and is centrifuged
Separate, 10-12 hours are vacuum dried at 80-85 DEG C will be deposited in, obtain amination barium titanate；
（5）Above-mentioned diatomite is calcined into 1-2 hours at 650-700 DEG C, normal temperature is cooled to, is mixed with above-mentioned polyethylene glycol, risen
High-temperature is 47-50 DEG C, in being added to the deionized water of compound weight 5-8 times, insulated and stirred 20-30 minute, obtains diatomite
Dispersion liquid；
（6）Above-mentioned amination barium titanate is added in the 1-METHYLPYRROLIDONE of its weight 10-17 times, is stirred, added
Above-mentioned 3,5- diaminobenzoic acids, ultrasonically treated 10-20 minutes, sequentially add above-mentioned lithium chloride, triphenyl phosphite, pyridine,
Nitrogen is passed through, the insulation reaction 3-4 hour in 100-105 DEG C of oil bath, discharging mixes with above-mentioned diatomite dispersion liquid, stirs
Uniformly, centrifugation, is vacuum dried 10-12 hours at being deposited in 80-85 DEG C, obtain polymer overmold barium titanate；
（7）Above-mentioned Kynoar is added in the dimethylformamide of its weight 4-6 times, the insulated and stirred at 80-90 DEG C
30-40 minutes, obtain amide solution；
（8）Take above-mentioned polymer overmold barium titanate, in being added to the dimethylformamide of its weight 4-6 times, ultrasonically treated 20-30
Minute, mix with above-mentioned amide solution and remaining each raw material, complete, the compacting at 176-180 DEG C is vacuum dried at 80-90 DEG C
Shaping, 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 then the present invention adopts 3,5 diaminourea
Preparing ultrabranching polyamide, triphenyl phosphite and pyridine serve as condensing agent to the method for benzoic acid polycondensation, and lithium chloride is then made
For the accelerator of solvability, because the amido link in lithium ion and polymer interacts, the hydrogen between polymer is reduced
Key is acted on, and so as in barium titanate nano particle surface grafting ultrabranching polyamide, and is grafted to the hyperbranched poly on barium titanate surface
Amide terminal has substantial amounts of free functional groups-NH2 so that composite nanometer particle has preferable electric conductivity, increase filler and
The difference of electrical conductivity between polymeric matrix, promotes the increase of interfacial polarization, or even, there is part-NH2 to be transformed into-NH3+,
Causing the electric conductivity of composite nanometer particle can further increase, so that interfacial polarization is also further enhanced；
The present invention inserts one layer in the middle of barium titanate and polyvinylidene fluoride resin matrix and has high dielectric constant and conductance
Ultrabranching polyamide, this aspect can increase the thickness of boundary layer, on the other hand can improve electric charge in interface zone
Transfer ability, so as to electric charge can be promoted to assemble in interface, strengthens interfacial polarization, improves the dielectric constant of composite.This
Bright with aluminium isopropoxide as presoma, obtained Alumina gel can effectively improve the compatibility of each storeroom, improve the table of finished product
Face resistance and stability.
Specific embodiment
A kind of Alumina gel high dielectric material, it is made up of the raw material of following weight parts：
Barium titanate 60, the diaminobenzoic acid 2.6 of gamma-aminopropyl-triethoxy-silane 10,3,5, triphenyl phosphite 6, pyridine 3,
Lithium chloride 0.02, cuprous bromide 4.3, Kynoar 7, HMPA 0.4, aluminium isopropoxide 4, dibutyl maleate 2,
Alkenyl succinic anhydride 0.2, dibutyl tin laurate 0.3, polyethylene glycol 3, dialkyl group are to biphenol 0.6, diatomite 2.
A kind of preparation method of described Alumina gel high dielectric material, comprises the following steps：
（1）Above-mentioned aluminium isopropoxide is added in the deionized water of 27 times of its weight, is stirred, it is 61 DEG C to rise high-temperature, is protected
Temperature stirring 10 minutes, adds above-mentioned alkenyl succinic anhydride, continues insulated and stirred 30 minutes, and the NaOH of 5mol/l is added dropwise, and adjusts
Section pH is 11, and the slow temperature that reduces is 36 DEG C, and insulated and stirred 18 minutes adds above-mentioned HMPA, stirs to normal temperature,
In being sent to baking oven, it is dried completely at 85 DEG C, obtains modified Alumina gel；
（2）Above-mentioned barium titanate 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 titanate；
（3）Above-mentioned dialkyl group is added in the absolute ethyl alcohol of 37 times of its weight to biphenol, is stirred, it is 60 to rise high-temperature
DEG C, insulated and stirred 10 minutes adds above-mentioned modified Alumina gel, ultrasound 3 minutes to obtain colloidal sol alcohol liquid；
（4）Above-mentioned hydroxylating barium titanate is added in absolute ethyl alcohol, ultrasound 6 minutes adds above-mentioned γ aminopropyl-triethoxies
Silane, is passed through nitrogen, insulated and stirred 20 hours at 76 DEG C, adds above-mentioned colloidal sol alcohol liquid, stirs, centrifugation, will be heavy
Form sediment and be vacuum dried 10 hours at 80 DEG C, obtain amination barium titanate；
（5）Above-mentioned diatomite is calcined 1 hour at 650 DEG C, normal temperature is cooled to, is mixed with above-mentioned polyethylene glycol, rise high-temperature
For 47 DEG C, in being added to the deionized water of 5 times of compound weight, insulated and stirred 20 minutes obtains diatomite dispersion liquid；
（6）Above-mentioned amination barium titanate is added in the N methyl pyrrolidones of 10 times of its weight, is stirred, added above-mentioned
3,5 diaminobenzoic acids, ultrasonically treated 10 minutes, sequentially add above-mentioned lithium chloride, triphenyl phosphite, pyridine, are passed through nitrogen,
Insulation reaction 3 hours in 100 DEG C of oil bath, discharging, mix with above-mentioned diatomite dispersion liquid, stir, centrifugation, will
It is vacuum dried 10 hours at being deposited in 80 DEG C, obtains polymer overmold barium titanate；
（7）Above-mentioned Kynoar is added in the dimethylformamide of 4 times of its weight, 30 points of insulated and stirred at 80 DEG C
Clock, obtains amide solution；
（8）Above-mentioned polymer overmold barium titanate is taken, in being added to the dimethylformamide of 4 times of its weight, ultrasonically treated 20 minutes,
Mix with above-mentioned amide solution and remaining each raw material, be vacuum dried completely at 80 DEG C, compressing at 176 DEG C, pressure is
In 20MPa.
The dielectric constant of composite of the present invention is 1453.6 in 1 kHz.
Claims (2)
1. a kind of Alumina gel high dielectric material, it is characterised in that it is made up of the raw material of following weight parts：
Barium titanate 60-75, gamma-aminopropyl-triethoxy-silane 10-14,3,5- diaminobenzoic acid 2.6-3, triphenyl phosphite
6-8, pyridine 3-4, lithium chloride 0.02-0.03, cuprous bromide 4.3-5, Kynoar 7-10, HMPA 0.4-1,
Aluminium isopropoxide 4-5, dibutyl maleate 2-3, alkenyl succinic anhydride 0.2-0.5, dibutyl tin laurate 0.3-1, poly- second two
Alcohol 3-4, dialkyl group are to biphenol 0.6-1, diatomite 2-4.
2. a kind of preparation method of Alumina gel high dielectric material as claimed in claim 1, it is characterised in that including following step
Suddenly：
（1）Above-mentioned aluminium isopropoxide is added in the deionized water of its weight 27-30 times, is stirred, liter high-temperature is 61-70
DEG C, insulated and stirred 10-15 minute, above-mentioned alkenyl succinic anhydride is added, continue insulated and stirred 30-40 minute, 5-7mol/l is added dropwise
NaOH, regulation pH is 11-13, and the slow temperature that reduces is 36-40 DEG C, insulated and stirred 18-20 minute, adds above-mentioned pregnancy
Base phosphoric triamide, stirs to normal temperature, in being sent to baking oven, is dried completely at 85-90 DEG C, obtains modified Alumina gel；
（2）Above-mentioned barium titanate 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 titanate；
（3）Above-mentioned dialkyl group is added in the absolute ethyl alcohol of its weight 37-40 times to biphenol, is stirred, rise high-temperature
For 60-64 DEG C, insulated and stirred 10-14 minute, above-mentioned modified Alumina gel is added, ultrasonic 3-4 minutes, obtain colloidal sol alcohol liquid；
（4）Above-mentioned hydroxylating barium titanate is added in absolute ethyl alcohol, ultrasonic 6-10 minutes, adds the above-mentioned second of γ-aminopropyl three
TMOS, is passed through nitrogen, the insulated and stirred 20-25 hour at 76-80 DEG C, adds above-mentioned colloidal sol alcohol liquid, stirs, and is centrifuged
Separate, 10-12 hours are vacuum dried at 80-85 DEG C will be deposited in, obtain amination barium titanate；
（5）Above-mentioned diatomite is calcined into 1-2 hours at 650-700 DEG C, normal temperature is cooled to, is mixed with above-mentioned polyethylene glycol, risen
High-temperature is 47-50 DEG C, in being added to the deionized water of compound weight 5-8 times, insulated and stirred 20-30 minute, obtains diatomite
Dispersion liquid；
（6）Above-mentioned amination barium titanate is added in the 1-METHYLPYRROLIDONE of its weight 10-17 times, is stirred, added
Above-mentioned 3,5- diaminobenzoic acids, ultrasonically treated 10-20 minutes, sequentially add above-mentioned lithium chloride, triphenyl phosphite, pyridine,
Nitrogen is passed through, the insulation reaction 3-4 hour in 100-105 DEG C of oil bath, discharging mixes with above-mentioned diatomite dispersion liquid, stirs
Uniformly, centrifugation, is vacuum dried 10-12 hours at being deposited in 80-85 DEG C, obtain polymer overmold barium titanate；
（7）Above-mentioned Kynoar is added in the dimethylformamide of its weight 4-6 times, the insulated and stirred at 80-90 DEG C
30-40 minutes, obtain amide solution；
（8）Take above-mentioned polymer overmold barium titanate, in being added to the dimethylformamide of its weight 4-6 times, ultrasonically treated 20-30
Minute, mix with above-mentioned amide solution and remaining each raw material, complete, the compacting at 176-180 DEG C is vacuum dried at 80-90 DEG C
Shaping, pressure is in 20-30MPa.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN108276511A (en) * | 2018-02-06 | 2018-07-13 | 杨秀枝 | A kind of preparation process by hot-forming dielectric composite material |
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