CN106111028A - A kind of preparation method of microcapsule battery compound polyimide dielectric material - Google Patents
A kind of preparation method of microcapsule battery compound polyimide dielectric material Download PDFInfo
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- CN106111028A CN106111028A CN201610484376.3A CN201610484376A CN106111028A CN 106111028 A CN106111028 A CN 106111028A CN 201610484376 A CN201610484376 A CN 201610484376A CN 106111028 A CN106111028 A CN 106111028A
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- 239000003094 microcapsule Substances 0.000 title claims abstract description 33
- 239000004642 Polyimide Substances 0.000 title claims abstract description 17
- 229920001721 polyimide Polymers 0.000 title claims abstract description 17
- 239000003989 dielectric material Substances 0.000 title claims abstract description 15
- 238000002360 preparation method Methods 0.000 title claims abstract description 15
- 150000001875 compounds Chemical class 0.000 title claims abstract description 11
- PAYRUJLWNCNPSJ-UHFFFAOYSA-N Aniline Chemical compound NC1=CC=CC=C1 PAYRUJLWNCNPSJ-UHFFFAOYSA-N 0.000 claims abstract description 21
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims abstract description 8
- 238000006277 sulfonation reaction Methods 0.000 claims abstract description 8
- 150000003233 pyrroles Chemical class 0.000 claims abstract description 7
- 238000003756 stirring Methods 0.000 claims description 36
- 238000010438 heat treatment Methods 0.000 claims description 29
- ROOXNKNUYICQNP-UHFFFAOYSA-N ammonium persulfate Chemical compound [NH4+].[NH4+].[O-]S(=O)(=O)OOS([O-])(=O)=O ROOXNKNUYICQNP-UHFFFAOYSA-N 0.000 claims description 24
- 238000002156 mixing Methods 0.000 claims description 22
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 18
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 18
- 239000012065 filter cake Substances 0.000 claims description 18
- 238000001914 filtration Methods 0.000 claims description 17
- CTQNGGLPUBDAKN-UHFFFAOYSA-N O-Xylene Chemical compound CC1=CC=CC=C1C CTQNGGLPUBDAKN-UHFFFAOYSA-N 0.000 claims description 15
- 239000007788 liquid Substances 0.000 claims description 14
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 12
- 229910001870 ammonium persulfate Inorganic materials 0.000 claims description 12
- 229920001467 poly(styrenesulfonates) Polymers 0.000 claims description 12
- 239000011347 resin Substances 0.000 claims description 12
- 229920005989 resin Polymers 0.000 claims description 12
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(1+) nitrate Chemical compound [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 claims description 12
- NWUYHJFMYQTDRP-UHFFFAOYSA-N 1,2-bis(ethenyl)benzene;1-ethenyl-2-ethylbenzene;styrene Chemical compound C=CC1=CC=CC=C1.CCC1=CC=CC=C1C=C.C=CC1=CC=CC=C1C=C NWUYHJFMYQTDRP-UHFFFAOYSA-N 0.000 claims description 11
- 239000003456 ion exchange resin Substances 0.000 claims description 11
- 229920003303 ion-exchange polymer Polymers 0.000 claims description 11
- UHOVQNZJYSORNB-UHFFFAOYSA-N monobenzene Natural products C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 claims description 11
- 239000008187 granular material Substances 0.000 claims description 10
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 9
- 238000000034 method Methods 0.000 claims description 7
- SECXISVLQFMRJM-UHFFFAOYSA-N N-Methylpyrrolidone Chemical compound CN1CCCC1=O SECXISVLQFMRJM-UHFFFAOYSA-N 0.000 claims description 6
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N Phenol Chemical compound OC1=CC=CC=C1 ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 claims description 6
- 238000006243 chemical reaction Methods 0.000 claims description 6
- 229910052802 copper Inorganic materials 0.000 claims description 6
- 239000010949 copper Substances 0.000 claims description 6
- 238000007654 immersion Methods 0.000 claims description 6
- 239000004005 microsphere Substances 0.000 claims description 6
- 239000002105 nanoparticle Substances 0.000 claims description 6
- 229910052757 nitrogen Inorganic materials 0.000 claims description 6
- 229920005990 polystyrene resin Polymers 0.000 claims description 6
- 239000012508 resin bead Substances 0.000 claims description 6
- 229910001961 silver nitrate Inorganic materials 0.000 claims description 6
- 235000011149 sulphuric acid Nutrition 0.000 claims description 6
- 239000001117 sulphuric acid Substances 0.000 claims description 6
- SRPWOOOHEPICQU-UHFFFAOYSA-N trimellitic anhydride Chemical compound OC(=O)C1=CC=C2C(=O)OC(=O)C2=C1 SRPWOOOHEPICQU-UHFFFAOYSA-N 0.000 claims description 6
- 239000003643 water by type Substances 0.000 claims description 6
- 239000000701 coagulant Substances 0.000 claims description 4
- 125000002490 anilino group Chemical group [H]N(*)C1=C([H])C([H])=C([H])C([H])=C1[H] 0.000 claims description 3
- 239000007789 gas Substances 0.000 claims description 3
- 239000008096 xylene Substances 0.000 claims description 3
- XZMCDFZZKTWFGF-UHFFFAOYSA-N Cyanamide Chemical compound NC#N XZMCDFZZKTWFGF-UHFFFAOYSA-N 0.000 claims description 2
- -1 benzene Ester Chemical class 0.000 claims description 2
- WFKAJVHLWXSISD-UHFFFAOYSA-N isobutyramide Chemical compound CC(C)C(N)=O WFKAJVHLWXSISD-UHFFFAOYSA-N 0.000 claims description 2
- 239000000463 material Substances 0.000 abstract description 7
- 239000002131 composite material Substances 0.000 abstract description 6
- 238000011068 loading method Methods 0.000 abstract description 4
- 230000007547 defect Effects 0.000 abstract description 3
- 239000000945 filler Substances 0.000 abstract description 3
- 239000004793 Polystyrene Substances 0.000 abstract description 2
- 230000007613 environmental effect Effects 0.000 abstract description 2
- 229920002223 polystyrene Polymers 0.000 abstract description 2
- 239000000243 solution Substances 0.000 description 28
- 239000000203 mixture Substances 0.000 description 9
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 6
- 238000005406 washing Methods 0.000 description 5
- 239000008367 deionised water Substances 0.000 description 4
- 229910021641 deionized water Inorganic materials 0.000 description 4
- DGTNSSLYPYDJGL-UHFFFAOYSA-N phenyl isocyanate Chemical compound O=C=NC1=CC=CC=C1 DGTNSSLYPYDJGL-UHFFFAOYSA-N 0.000 description 4
- 238000011161 development Methods 0.000 description 3
- 239000006185 dispersion Substances 0.000 description 3
- KAESVJOAVNADME-UHFFFAOYSA-N Pyrrole Chemical compound C=1C=CNC=1 KAESVJOAVNADME-UHFFFAOYSA-N 0.000 description 2
- 150000001412 amines Chemical class 0.000 description 2
- 239000007864 aqueous solution Substances 0.000 description 2
- 239000002305 electric material Substances 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 125000001997 phenyl group Chemical group [H]C1=C([H])C([H])=C(*)C([H])=C1[H] 0.000 description 2
- 238000012827 research and development Methods 0.000 description 2
- 206010011224 Cough Diseases 0.000 description 1
- 239000004952 Polyamide Substances 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 238000006731 degradation reaction Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000005684 electric field Effects 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 238000013467 fragmentation Methods 0.000 description 1
- 238000006062 fragmentation reaction Methods 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 238000004377 microelectronic Methods 0.000 description 1
- 229920002647 polyamide Polymers 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 238000006116 polymerization reaction Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 230000000630 rising effect Effects 0.000 description 1
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J13/00—Colloid chemistry, e.g. the production of colloidal materials or their solutions, not otherwise provided for; Making microcapsules or microballoons
- B01J13/02—Making microcapsules or microballoons
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J13/00—Colloid chemistry, e.g. the production of colloidal materials or their solutions, not otherwise provided for; Making microcapsules or microballoons
- B01J13/0052—Preparation of gels
- B01J13/0065—Preparation of gels containing an organic phase
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G73/00—Macromolecular compounds obtained by reactions forming a linkage containing nitrogen with or without oxygen or carbon in the main chain of the macromolecule, not provided for in groups C08G12/00 - C08G71/00
- C08G73/06—Polycondensates having nitrogen-containing heterocyclic rings in the main chain of the macromolecule
- C08G73/0605—Polycondensates containing five-membered rings, not condensed with other rings, with nitrogen atoms as the only ring hetero atoms
- C08G73/0611—Polycondensates containing five-membered rings, not condensed with other rings, with nitrogen atoms as the only ring hetero atoms with only one nitrogen atom in the ring, e.g. polypyrroles
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Dispersion Chemistry (AREA)
- Health & Medical Sciences (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Battery Electrode And Active Subsutance (AREA)
- Macromolecular Compounds Obtained By Forming Nitrogen-Containing Linkages In General (AREA)
- Compositions Of Macromolecular Compounds (AREA)
- Secondary Cells (AREA)
Abstract
The present invention relates to the preparation method of a kind of microcapsule battery compound polyimide dielectric material, belong to dielectric material preparing technical field.The polymide dielectric composite dielectric loss that the present invention is directed to prepare at present is the biggest, and during high filler loading capacity, cause the defect that its mechanical property declines to a great extent, a kind of by by polystyrene sulfonation, it is polymerized with pyrroles again and prepares hollow microcapsules, fill a vacancy inside its microcapsule by aniline subsequently, silver-plated by nano surface copper powder again, form the battery structure of a kind of microcapsule formula, by microcapsule battery filled polyimide material, while its dielectric constant is greatly improved, it is effectively improved toughness and the intensity of polyimides, microcapsule battery compound polyimide dielectric material dielectric constant prepared by the present invention is up to 135, and impact strength is up to 280KJ/m2, and preparation process is simple, environmental protection, environmentally safe.
Description
Technical field
The present invention relates to the preparation method of a kind of microcapsule battery compound polyimide dielectric material, belong to dielectric material system
Standby technical field.
Background technology
High electric material is a kind of application prospect insulant widely, well stores electric energy with equal owing to it has
The performance of even electric field, thus in electronics, motor and cable industry, have very important application.Polyimides is based on excellence
The advantage that other polymer such as hot property, mechanical performance and dielectric properties are incomparable, in microelectronics high-tech area and aviation
Space industry is extensively applied.Due to the designability in its structure, increasing researcher puts into this kind of high skill in the world
In the research and development of art material.But along with the research of material is constantly towards high performance, multifunction and cost degradation direction
Development.In view of a little self such as hygroscopicity and the more high weak point of thermal coefficient of expansion, along with science and technology and the development of industrial or agricultural, electric
Gas and the miniaturization of motor device and miniature development, frequency control and high-pressure trend require need to constantly put forward the performance of insulant
Rising, simple polyimide material is requiring the Material Field of specific function, for the application performance modification improved with this
Exploitation for the composite of matrix is always academia and the focus of industrial quarters research and development with application.
Although existing modification prepare polymide dielectric composite study ratio is wide, but to reach the highest Jie
Electric constant, the filler loading generally used will be the highest.On the one hand this make the dielectric loss of composite very greatly, and
When loading is too high, drawing abillity also can become very poor, it is easy to fragmentation.So needing a kind of effective polyamides sub-
Amine dielectric material is necessary.
Summary of the invention
The technical problem to be solved: for the polymide dielectric composite dielectric loss prepared at present very
Greatly, the defect that its mechanical property declines to a great extent and is caused during high filler loading capacity, it is provided that a kind of by by polystyrene sulfonation, then with
Hollow microcapsules is prepared in pyrroles's polymerization, fills a vacancy inside its microcapsule by aniline subsequently, more silver-plated by nano surface copper powder, shape
Become the battery structure of a kind of microcapsule formula, by microcapsule battery filled polyimide material, its dielectric constant is being greatly improved
While, it is effectively improved toughness and the intensity of polyimides, effectively solves polymide dielectric composite dielectric loss
Greatly, the defect of poor mechanical property.
For solving above-mentioned technical problem, the present invention uses the technical scheme as described below to be:
(1) 1:5 in mass ratio, mixes polystyrene resin beads, 200～300W with the stirring of mass concentration 85% concentrated sulphuric acid
Lower ultrasonic disperse processes so that it is after sulfonation 10～15min, sucking filtration also collects filter cake, washs 3 with mass concentration 10% sulfuric acid solution
～after 5 times, then be washed with deionized 3～5 times, at 65～80 DEG C, it is dried 6～8h, is prepared into sulfonated polystyrene ion exchange resin
Grain；
(2) count by weight, weigh 5～10 parts of mass concentration 20% ammonium persulfate solutions, 25～30 parts of above-mentioned preparations respectively
Sulfonated polystyrene ion exchange resin granule, 5～10 parts of copper nanoparticles and 45～60 parts of deionized waters are placed in there-necked flask, stirring mixing
It is placed at 65～80 DEG C preheating 25～30min；
(3) after preheating completes, to its dropping ammonium persulfate solution pyrroles identical in quality, control time for adding be 10～
15min, after being added dropwise to complete, then heating in water bath 20～24h at 20～30 DEG C, it is prepared into conductive hollow microsphere, in mass ratio
1:10, is placed in conductive micro-balloons and aniline solution in beaker, and stirring mixing also soaks 20～24h；
(4) after immersion completes, to the silver nitrate solution of dropping mass concentration 10% in beaker, control dripping quantity is aniline solution
1/2, after being added dropwise to complete, then ultrasonic disperse 15～20min under 200～300W, sucking filtration collect filter cake subsequently, naturally dry in the air
The dry microcapsule battery resin that is prepared into, standby；
(5) count by weight, weigh 30～35 parts of N-Methyl pyrrolidone, 15～20 parts of dimethylbenzene, 5～10 parts of N ' N-respectively
Dimethyl acetylamide and 25～30 parts of N ' dinethylformamides are placed in there-necked flask stirring mixing, lead to nitrogen subsequently and get rid of sky
Gas, is placed in oil bath heating 45～60min at 120～125 DEG C by there-necked flask；
(6) to be heated complete after, there-necked flask is added respectively the trimellitic anhydride identical with xylene mass and Carbimide. benzene
Ester, to be added complete after, stirring mixing also heats up and is placed at 180～185 DEG C oil bath heating 25～30min, is prepared into middle mixed
Close liquid；
(7) 1:1:8 in mass ratio, microcapsule battery resin step (4) prepared, phenol add successively to middle mixed liquor
In, to be added complete after, be continuously heating to 200～210 DEG C of oil baths heating, after reaction 1～2h to be heated, collect while hot and to obtain mixing
Coagulant liquid；
(8) 1:10 in mass ratio, mixes 10～15min by mixed gel liquid with methanol stirring, stands and be cooled to sucking filtration after room temperature
And collect filter cake, after being washed with deionized 3～5 times, it is placed at 65～80 DEG C and is dried 6～8h, one can be prepared into
Microcapsule battery compound polyimide dielectric material.
Polymide dielectric tensile strength of material prepared by the present invention is up to 58～65MPa, and dielectric constant reaches as high as
135, and impact strength is up to 261KJ/m2。
The present invention is compared with additive method, and Advantageous Effects is:
(1) the microcapsule battery compound polyimide dielectric material dielectric constant that prepared by the present invention is up to 135, and impact strength
Up to 280KJ/m2；
(2) preparation process of the present invention is simple, environmental protection, environmentally safe.
Detailed description of the invention
1:5 the most in mass ratio, mixes the stirring of polystyrene resin beads and mass concentration 85% concentrated sulphuric acid, 200～
Under 300W, ultrasonic disperse processes so that it is after sulfonation 10～15min, sucking filtration also collects filter cake, washes with mass concentration 10% sulfuric acid solution
After washing 3～5 times, then it is washed with deionized 3～5 times, at 65～80 DEG C, is dried 6～8h, is prepared into sulfonated polystyrene tree
Fat granule；Count by weight, weigh 5～10 parts of mass concentration 20% ammonium persulfate solutions, 25～30 parts of above-mentioned preparations respectively
Sulfonated polystyrene ion exchange resin granule, 5～10 parts of copper nanoparticles and 45～60 parts of deionized waters are placed in there-necked flask, stirring mixing
It is placed at 65～80 DEG C preheating 25～30min；After preheating completes, the pyrrole identical in quality to its dropping ammonium persulfate solution
Coughing up, controlling time for adding is 10～15min, after being added dropwise to complete, then heating in water bath 20～24h at 20～30 DEG C, it is prepared into
Conductive hollow microsphere, in mass ratio 1:10, be placed in conductive micro-balloons and aniline solution in beaker, stirring mixing and soak 20～
24h；After immersion completes, to the silver nitrate solution of dropping mass concentration 10% in beaker, controlling dripping quantity is the 1/ of aniline solution
2, after being added dropwise to complete, then ultrasonic disperse 15～20min under 200～300W, sucking filtration collect filter cake subsequently, dries system naturally
The standby microcapsule battery resin that obtains, standby；Count by weight, weigh respectively 30～35 parts of N-Methyl pyrrolidone, 15～20 parts
Dimethylbenzene, 5～10 parts of N ' N-dimethyl acetylamide and 25～30 parts of N ' dinethylformamides are placed in there-necked flask stirring and mix
Close, lead to nitrogen subsequently and get rid of air, there-necked flask is placed in oil bath heating 45～60min at 120～125 DEG C；To be heated complete
After, there-necked flask is added respectively the trimellitic anhydride identical with xylene mass and carbanil, to be added complete after, stir
Mix mixing and intensification is placed in oil bath heating 25～30min at 180～185 DEG C, be prepared into middle mixed liquor；1:1:8 in mass ratio,
The microcapsule battery resin step (4) prepared, phenol add successively to middle mixed liquor, to be added complete after, continue to rise
Temperature, to 200～210 DEG C of oil bath heating, after reaction 1～2h to be heated, collects to obtain mixed gel liquid while hot；1:10 in mass ratio, will
The stirring of mixed gel liquid and methanol mix 10～15min, standing be cooled to room temperature after sucking filtration collect filter cake, be washed with deionized water
After washing 3～5 times, it is placed at 65～80 DEG C and is dried 6～8h, a kind of microcapsule battery compound polyimide can be prepared into and be situated between
Electric material.
Example 1
1:5 the most in mass ratio, mixes polystyrene resin beads with the stirring of mass concentration 85% concentrated sulphuric acid, super under 200W
Sound dispersion processes so that it is after sulfonation 10min, sucking filtration also collects filter cake, after washing 3 times with mass concentration 10% sulfuric acid solution, then uses
Deionized water wash 3 times, is dried 6h at 65 DEG C, is prepared into sulfonated polystyrene ion exchange resin granule；Count by weight, claim respectively
Measure 5 parts of mass concentration 20% ammonium persulfate solutions, the sulfonated polystyrene ion exchange resin granule of 30 parts of above-mentioned preparations, 10 parts of copper nanoparticles
Being placed in there-necked flask with 60 parts of deionized waters, stirring mixing is placed at 65 DEG C preheating 25min；After preheating completes, to it
The pyrroles that dropping ammonium persulfate solution is identical in quality, control time for adding is 10min, after being added dropwise to complete, then water at 20 DEG C
Bath heating 20h, is prepared into conductive hollow microsphere, in mass ratio 1:10, conductive micro-balloons and aniline solution is placed in beaker, stirring
Mix and soak 20h；After immersion completes, to the silver nitrate solution of dropping mass concentration 10% in beaker, control dripping quantity is benzene
The 1/2 of amine aqueous solution, after being added dropwise to complete, then ultrasonic disperse 15min under 200W, sucking filtration collect filter cake subsequently, dries naturally
It is prepared into microcapsule battery resin, standby；Count by weight, weigh respectively 30 parts of N-Methyl pyrrolidone, 15 parts of dimethylbenzene,
5 parts of N ' N-dimethyl acetylamide and 25 parts of N ' dinethylformamides are placed in there-necked flask stirring mixing, lead to nitrogen row subsequently
Except air, there-necked flask is placed in oil bath heating 45min at 120 DEG C；To be heated complete after, there-necked flask is added respectively with two
Trimellitic anhydride that toluene is identical in quality and carbanil, to be added complete after, stirring mixing also heats up and is placed at 180 DEG C oil
Bath heating 25min, is prepared into middle mixed liquor；1:1:8 in mass ratio, microcapsule battery resin, phenol are added successively in
Between in mixed liquor, to be added complete after, be continuously heating to 200 DEG C of oil baths heating, after reaction 1h to be heated, collect while hot to obtain and mix
Coagulant liquid；1:10 in mass ratio, mix 10min by the stirring of mixed gel liquid and methanol, standing be cooled to room temperature after sucking filtration receiving
Collection filter cake, after being washed with deionized 3 times, is placed at 65 DEG C and is dried 6h, can be prepared into a kind of microcapsule battery and be combined
Polymide dielectric material.
Example 2
1:5 the most in mass ratio, mixes polystyrene resin beads with the stirring of mass concentration 85% concentrated sulphuric acid, super under 250W
Sound dispersion processes so that it is after sulfonation 12min, sucking filtration also collects filter cake, after washing 4 times with mass concentration 10% sulfuric acid solution, then uses
Deionized water wash 4 times, is dried 7h at 70 DEG C, is prepared into sulfonated polystyrene ion exchange resin granule；Count by weight, claim respectively
Measure 7 parts of mass concentration 20% ammonium persulfate solutions, the sulfonated polystyrene ion exchange resin granule of 22 parts of above-mentioned preparations, 8 parts of copper nanoparticles and
50 parts of deionized waters are placed in there-necked flask, and stirring mixing is placed at 70 DEG C preheating 27min；After preheating completes, to it
Adding the pyrroles that ammonium persulfate solution is identical in quality, control time for adding is 12min, after being added dropwise to complete, then water-bath at 25 DEG C
Heating 22h, is prepared into conductive hollow microsphere, in mass ratio 1:10, conductive micro-balloons and aniline solution is placed in beaker, and stirring is mixed
Merge and soak 22h；After immersion completes, to the silver nitrate solution of dropping mass concentration 10% in beaker, control dripping quantity is aniline
The 1/2 of solution, after being added dropwise to complete, then ultrasonic disperse 17min under 250W, sucking filtration collect filter cake subsequently, dries system naturally
The standby microcapsule battery resin that obtains, standby；Count by weight, weigh respectively 32 parts of N-Methyl pyrrolidone, 17 parts of dimethylbenzene, 8
Part N ' N-dimethyl acetylamide and 27 parts of N ' dinethylformamides are placed in there-necked flask stirring mixing, lead to nitrogen subsequently and get rid of
Air, is placed in oil bath heating 50min at 122 DEG C by there-necked flask；To be heated complete after, there-necked flask is added and diformazan respectively
Trimellitic anhydride that benzene is identical in quality and carbanil, to be added complete after, stirring mixing also heats up and is placed in oil bath at 182 DEG C
Heating 27min, is prepared into middle mixed liquor；1:1:8 in mass ratio, adds successively by the microcapsule battery resin of preparation, phenol
To middle mixed liquor, to be added complete after, be continuously heating to 205 DEG C of oil baths heating, after reaction 1.5h to be heated, collect while hot
Obtain mixed gel liquid；1:10 in mass ratio, mixes 12min by mixed gel liquid with methanol stirring, stands and takes out after being cooled to room temperature
Filter and collect filter cake, after being washed with deionized 4 times, being placed at 70 DEG C and be dried 7h, a kind of microcapsule electricity can be prepared into
Pond compound polyimide dielectric material.
Example 3
1:5 the most in mass ratio, mixes polystyrene resin beads with the stirring of mass concentration 85% concentrated sulphuric acid, super under 300W
Sound dispersion processes so that it is after sulfonation 15min, sucking filtration also collects filter cake, after washing 5 times with mass concentration 10% sulfuric acid solution, then uses
Deionized water wash 5 times, is dried 8h at 80 DEG C, is prepared into sulfonated polystyrene ion exchange resin granule；Count by weight, claim respectively
Measure 10 parts of mass concentration 20% ammonium persulfate solutions, the sulfonated polystyrene ion exchange resin granule of 30 parts of above-mentioned preparations, 10 parts of copper nanoparticles
Being placed in there-necked flask with 60 parts of deionized waters, stirring mixing is placed at 80 DEG C preheating 30min；After preheating completes, to it
The pyrroles that dropping ammonium persulfate solution is identical in quality, control time for adding is 15min, after being added dropwise to complete, then water at 30 DEG C
Bath heating 24h, is prepared into conductive hollow microsphere, in mass ratio 1:10, conductive micro-balloons and aniline solution is placed in beaker, stirring
Mix and soak 24h；After immersion completes, to the silver nitrate solution of dropping mass concentration 10% in beaker, control dripping quantity is benzene
The 1/2 of amine aqueous solution, after being added dropwise to complete, then ultrasonic disperse 20min under 300W, sucking filtration collect filter cake subsequently, dries naturally
It is prepared into microcapsule battery resin, standby；Count by weight, weigh respectively 35 parts of N-Methyl pyrrolidone, 20 parts of dimethylbenzene,
10 parts of N ' N-dimethyl acetylamide and 30 parts of N ' dinethylformamides are placed in there-necked flask stirring mixing, lead to nitrogen row subsequently
Except air, there-necked flask is placed in oil bath heating 60min at 125 DEG C；To be heated complete after, there-necked flask is added respectively with two
Trimellitic anhydride that toluene is identical in quality and carbanil, to be added complete after, stirring mixing also heats up and is placed at 185 DEG C oil
Bath heating 30min, is prepared into middle mixed liquor；1:1:8 in mass ratio, microcapsule battery resin, phenol are added successively in
Between in mixed liquor, to be added complete after, be continuously heating to 210 DEG C of oil baths heating, after reaction 2h to be heated, collect while hot to obtain and mix
Coagulant liquid；1:10 in mass ratio, mix 15min by the stirring of mixed gel liquid and methanol, standing be cooled to room temperature after sucking filtration receiving
Collection filter cake, after being washed with deionized 5 times, is placed at 80 DEG C and is dried 8h, can be prepared into a kind of microcapsule battery and be combined
Polymide dielectric material.
Claims (1)
1. the preparation method of a microcapsule battery compound polyimide dielectric material, it is characterised in that concrete preparation process is:
(1) 1:5 in mass ratio, mixes polystyrene resin beads, 200～300W with the stirring of mass concentration 85% concentrated sulphuric acid
Lower ultrasonic disperse processes so that it is after sulfonation 10～15min, sucking filtration also collects filter cake, washs 3 with mass concentration 10% sulfuric acid solution
～after 5 times, then be washed with deionized 3～5 times, at 65～80 DEG C, it is dried 6～8h, is prepared into sulfonated polystyrene ion exchange resin
Grain；
(2) count by weight, weigh 5～10 parts of mass concentration 20% ammonium persulfate solutions, 25～30 parts of above-mentioned preparations respectively
Sulfonated polystyrene ion exchange resin granule, 5～10 parts of copper nanoparticles and 45～60 parts of deionized waters are placed in there-necked flask, stirring mixing
It is placed at 65～80 DEG C preheating 25～30min；
(3) after preheating completes, to its dropping ammonium persulfate solution pyrroles identical in quality, control time for adding be 10～
15min, after being added dropwise to complete, then heating in water bath 20～24h at 20～30 DEG C, it is prepared into conductive hollow microsphere, in mass ratio
1:10, is placed in conductive micro-balloons and aniline solution in beaker, and stirring mixing also soaks 20～24h；
(4) after immersion completes, to the silver nitrate solution of dropping mass concentration 10% in beaker, control dripping quantity is aniline solution
1/2, after being added dropwise to complete, then ultrasonic disperse 15～20min under 200～300W, sucking filtration collect filter cake subsequently, naturally dry in the air
The dry microcapsule battery resin that is prepared into, standby；
(5) count by weight, weigh 30～35 parts of N-Methyl pyrrolidone, 15～20 parts of dimethylbenzene, 5～10 parts of N ' N-respectively
Dimethyl acetylamide and 25～30 parts of N ' dinethylformamides are placed in there-necked flask stirring mixing, lead to nitrogen subsequently and get rid of sky
Gas, is placed in oil bath heating 45～60min at 120～125 DEG C by there-necked flask；
(6) to be heated complete after, there-necked flask is added respectively the trimellitic anhydride identical with xylene mass and Carbimide. benzene
Ester, to be added complete after, stirring mixing also heats up and is placed at 180～185 DEG C oil bath heating 25～30min, is prepared into middle mixed
Close liquid；
(7) 1:1:8 in mass ratio, microcapsule battery resin step (4) prepared, phenol add successively to middle mixed liquor
In, to be added complete after, be continuously heating to 200～210 DEG C of oil baths heating, after reaction 1～2h to be heated, collect while hot and to obtain mixing
Coagulant liquid；
(8) 1:10 in mass ratio, mixes 10～15min by mixed gel liquid with methanol stirring, stands and be cooled to sucking filtration after room temperature
And collect filter cake, after being washed with deionized 3～5 times, it is placed at 65～80 DEG C and is dried 6～8h, one can be prepared into
Microcapsule battery compound polyimide dielectric material.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN108975797A (en) * | 2018-09-17 | 2018-12-11 | 佛山朝鸿新材料科技有限公司 | A kind of preparation method of ultralight foam concrete |
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