CN117164857A - Intrinsic high-dielectric-property phosphine oxide polyimide and preparation method thereof - Google Patents
Intrinsic high-dielectric-property phosphine oxide polyimide and preparation method thereof Download PDFInfo
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- CN117164857A CN117164857A CN202311271093.7A CN202311271093A CN117164857A CN 117164857 A CN117164857 A CN 117164857A CN 202311271093 A CN202311271093 A CN 202311271093A CN 117164857 A CN117164857 A CN 117164857A
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- 229920001721 polyimide Polymers 0.000 title claims abstract description 56
- 239000004642 Polyimide Substances 0.000 title claims abstract description 53
- AUONHKJOIZSQGR-UHFFFAOYSA-N oxophosphane Chemical compound P=O AUONHKJOIZSQGR-UHFFFAOYSA-N 0.000 title abstract description 8
- 238000002360 preparation method Methods 0.000 title abstract description 8
- 238000000034 method Methods 0.000 claims abstract description 15
- XQUPVDVFXZDTLT-UHFFFAOYSA-N 1-[4-[[4-(2,5-dioxopyrrol-1-yl)phenyl]methyl]phenyl]pyrrole-2,5-dione Chemical compound O=C1C=CC(=O)N1C(C=C1)=CC=C1CC1=CC=C(N2C(C=CC2=O)=O)C=C1 XQUPVDVFXZDTLT-UHFFFAOYSA-N 0.000 claims abstract description 9
- MZRVEZGGRBJDDB-UHFFFAOYSA-N N-Butyllithium Chemical compound [Li]CCCC MZRVEZGGRBJDDB-UHFFFAOYSA-N 0.000 claims abstract description 8
- 229920003192 poly(bis maleimide) Polymers 0.000 claims abstract description 8
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 claims abstract description 6
- 239000003960 organic solvent Substances 0.000 claims abstract description 5
- GMHHTGYHERDNLO-UHFFFAOYSA-N 4-bromobicyclo[4.2.0]octa-1(6),2,4-triene Chemical compound BrC1=CC=C2CCC2=C1 GMHHTGYHERDNLO-UHFFFAOYSA-N 0.000 claims abstract description 4
- IMDXZWRLUZPMDH-UHFFFAOYSA-N dichlorophenylphosphine Chemical compound ClP(Cl)C1=CC=CC=C1 IMDXZWRLUZPMDH-UHFFFAOYSA-N 0.000 claims abstract description 4
- 238000010345 tape casting Methods 0.000 claims abstract description 3
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 claims description 15
- -1 phosphine benzocyclobutene Chemical compound 0.000 claims description 14
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims description 10
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 claims description 9
- 239000003153 chemical reaction reagent Substances 0.000 claims description 9
- 238000010438 heat treatment Methods 0.000 claims description 8
- 239000000126 substance Substances 0.000 claims description 8
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical group CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 6
- WYURNTSHIVDZCO-UHFFFAOYSA-N Tetrahydrofuran Chemical compound C1CCOC1 WYURNTSHIVDZCO-UHFFFAOYSA-N 0.000 claims description 6
- 239000003208 petroleum Substances 0.000 claims description 5
- 238000013007 heat curing Methods 0.000 claims description 4
- 239000007800 oxidant agent Substances 0.000 claims description 4
- 230000001590 oxidative effect Effects 0.000 claims description 4
- FXHOOIRPVKKKFG-UHFFFAOYSA-N N,N-Dimethylacetamide Chemical compound CN(C)C(C)=O FXHOOIRPVKKKFG-UHFFFAOYSA-N 0.000 claims description 3
- SECXISVLQFMRJM-UHFFFAOYSA-N N-Methylpyrrolidone Chemical compound CN1CCCC1=O SECXISVLQFMRJM-UHFFFAOYSA-N 0.000 claims description 3
- 238000006243 chemical reaction Methods 0.000 claims description 3
- 238000001035 drying Methods 0.000 claims description 3
- 238000002156 mixing Methods 0.000 claims description 3
- 239000000178 monomer Substances 0.000 claims description 3
- YLQBMQCUIZJEEH-UHFFFAOYSA-N tetrahydrofuran Natural products C=1C=COC=1 YLQBMQCUIZJEEH-UHFFFAOYSA-N 0.000 claims description 3
- TZJSKWSWPJBRBE-UHFFFAOYSA-N [P].C1CC=2C1=CC=CC2 Chemical compound [P].C1CC=2C1=CC=CC2 TZJSKWSWPJBRBE-UHFFFAOYSA-N 0.000 claims description 2
- 239000012046 mixed solvent Substances 0.000 claims 2
- 238000004587 chromatography analysis Methods 0.000 claims 1
- 238000004519 manufacturing process Methods 0.000 claims 1
- 239000000463 material Substances 0.000 abstract description 3
- 239000002861 polymer material Substances 0.000 abstract description 3
- 238000005698 Diels-Alder reaction Methods 0.000 abstract description 2
- 238000004377 microelectronic Methods 0.000 abstract description 2
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 abstract 2
- 229910052698 phosphorus Inorganic materials 0.000 abstract 2
- 239000011574 phosphorus Substances 0.000 abstract 2
- 238000004891 communication Methods 0.000 abstract 1
- 229960002163 hydrogen peroxide Drugs 0.000 abstract 1
- 238000002844 melting Methods 0.000 abstract 1
- 230000008018 melting Effects 0.000 abstract 1
- 239000005022 packaging material Substances 0.000 abstract 1
- 229920001187 thermosetting polymer Polymers 0.000 abstract 1
- 239000004634 thermosetting polymer Substances 0.000 abstract 1
- 230000004580 weight loss Effects 0.000 description 8
- 230000015572 biosynthetic process Effects 0.000 description 5
- 238000003786 synthesis reaction Methods 0.000 description 5
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 4
- 229910052799 carbon Inorganic materials 0.000 description 4
- 239000011521 glass Substances 0.000 description 4
- WFDIJRYMOXRFFG-UHFFFAOYSA-N Acetic anhydride Chemical compound CC(=O)OC(C)=O WFDIJRYMOXRFFG-UHFFFAOYSA-N 0.000 description 3
- RPGWZZNNEUHDAQ-UHFFFAOYSA-N phenylphosphine Chemical compound PC1=CC=CC=C1 RPGWZZNNEUHDAQ-UHFFFAOYSA-N 0.000 description 3
- 238000001029 thermal curing Methods 0.000 description 3
- XYFCBTPGUUZFHI-UHFFFAOYSA-N Phosphine Chemical compound P XYFCBTPGUUZFHI-UHFFFAOYSA-N 0.000 description 2
- HEDRZPFGACZZDS-MICDWDOJSA-N Trichloro(2H)methane Chemical compound [2H]C(Cl)(Cl)Cl HEDRZPFGACZZDS-MICDWDOJSA-N 0.000 description 2
- MVPPADPHJFYWMZ-UHFFFAOYSA-N chlorobenzene Chemical compound ClC1=CC=CC=C1 MVPPADPHJFYWMZ-UHFFFAOYSA-N 0.000 description 2
- 238000011097 chromatography purification Methods 0.000 description 2
- RLSSMJSEOOYNOY-UHFFFAOYSA-N m-cresol Chemical compound CC1=CC=CC(O)=C1 RLSSMJSEOOYNOY-UHFFFAOYSA-N 0.000 description 2
- 230000000630 rising effect Effects 0.000 description 2
- 239000002904 solvent Substances 0.000 description 2
- 238000003756 stirring Methods 0.000 description 2
- FYSNRJHAOHDILO-UHFFFAOYSA-N thionyl chloride Chemical compound ClS(Cl)=O FYSNRJHAOHDILO-UHFFFAOYSA-N 0.000 description 2
- 238000005160 1H NMR spectroscopy Methods 0.000 description 1
- RNFJDJUURJAICM-UHFFFAOYSA-N 2,2,4,4,6,6-hexaphenoxy-1,3,5-triaza-2$l^{5},4$l^{5},6$l^{5}-triphosphacyclohexa-1,3,5-triene Chemical compound N=1P(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP=1(OC=1C=CC=CC=1)OC1=CC=CC=C1 RNFJDJUURJAICM-UHFFFAOYSA-N 0.000 description 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- 239000012346 acetyl chloride Substances 0.000 description 1
- WETWJCDKMRHUPV-UHFFFAOYSA-N acetyl chloride Chemical compound CC(Cl)=O WETWJCDKMRHUPV-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- UMIVXZPTRXBADB-UHFFFAOYSA-N benzocyclobutene Chemical group C1=CC=C2CCC2=C1 UMIVXZPTRXBADB-UHFFFAOYSA-N 0.000 description 1
- CREMABGTGYGIQB-UHFFFAOYSA-N carbon carbon Chemical compound C.C CREMABGTGYGIQB-UHFFFAOYSA-N 0.000 description 1
- 239000011203 carbon fibre reinforced carbon Substances 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 238000012512 characterization method Methods 0.000 description 1
- 238000001723 curing Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 239000003063 flame retardant Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 239000005457 ice water Substances 0.000 description 1
- 150000003949 imides Chemical group 0.000 description 1
- 238000000655 nuclear magnetic resonance spectrum Methods 0.000 description 1
- 229910000073 phosphorus hydride Inorganic materials 0.000 description 1
- 229920005575 poly(amic acid) Polymers 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 238000003825 pressing Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 230000000979 retarding effect Effects 0.000 description 1
- 238000002390 rotary evaporation Methods 0.000 description 1
- 150000003384 small molecules Chemical class 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 238000010025 steaming Methods 0.000 description 1
Landscapes
- Macromolecular Compounds Obtained By Forming Nitrogen-Containing Linkages In General (AREA)
Abstract
The invention belongs to the technical field of high polymer materials, and particularly relates to a phosphine oxide polyimide with intrinsic high dielectric property and a preparation method thereof. Firstly, 4-bromobenzocyclobutene, n-butyllithium and phenyl phosphorus dichloride react, and then oxydol is oxidized to prepare phosphorus oxybenzocyclobutene; and then carrying out Diels-Alder reaction with bismaleimide to prepare the intrinsic high-dielectric-property phosphine oxide polyimide. The prepared phosphorus oxybenzocyclobutene has low melting point, is dissolved in most organic solvents, has excellent processing performance, can be melted and solidified with bismaleimide in a die, and can be prepared into a polyimide film by a tape casting method. The polyimide prepared by the invention has high thermal stability and high dielectric property due to the existence of phosphorus-oxygen double bonds with large polarity, and can be used as a thermosetting polymer material in the fields of 5G communication, microelectronics, packaging materials and the like.
Description
Technical Field
The invention belongs to the field of polymers, and particularly relates to an intrinsic high-dielectric-property phosphine oxide polyimide and a preparation method thereof.
Background
Polyimide (PI) is a high polymer material with high heat resistance, good chemical stability, excellent mechanical property and electrical property, which contains imide ring on the main chain, and is widely applied to the high and new technical fields of aviation, aerospace, electric, microelectronics, automobiles and the like. The traditional polyimide is prepared by a one-step chlorobenzene/m-cresol solvent method, or a two-step method: the polyamic acid is first formed in N, N-dimethylacetamide/N-methylpyrrolidone/N, N-dimethylformamide solvent and then subjected to thermal imidization (about 300 ℃) or chemical imidization with acetic anhydride/acetyl chloride/thionyl chloride reagent. The escape of moisture during thermal or chemical imidization can cause a film to undergo a large shrinkage, severely affecting the product properties. Therefore, the invention is very beneficial to the phosphine oxide polyimide with the intrinsic high dielectric property and the preparation method thereof.
Disclosure of Invention
The technical problems solved by the invention are as follows: an intrinsic phosphinic polyimide and its preparing process are disclosed, which features high thermal stability, high dielectric performance and flame retarding performance.
The invention solves the technical problems through the following technical scheme:
an intrinsic type phosphinic polyimide, the structural formula of which is shown as the following formula (1):
wherein n is a positive integer greater than 1, the theoretical number is not limited, and the specific value is determined by the amount of the raw material monomer cured in the previous step. Preferably n is 10000.
R in the structural formula (1) is selected from any one of the following structures:
the invention also provides a preparation method of the intrinsic type phosphinic polyimide, which comprises the following steps:
(1) Preparing a monomer: firstly, adding 4-bromobenzocyclobutene and N-butyllithium, N into anhydrous anaerobic reagent 2 Reacting for 5 hours at the temperature of minus 80 ℃, and adding phenyl dichlorophosphorus to react for 4 hours to obtain phosphine benzocyclobutene; in anhydrous reagent, adding oxidant into phosphorus benzocyclobutene to react for 20-28h, and passing petroleum ether: ethyl acetate = 10: and (3) performing chromatographic purification to obtain the phosphine oxide benzocyclobutene.
(2) And (3) a heat curing stage: mixing the phosphorus oxide benzocyclobutene prepared in the step (1) and bismaleimide according to a mass ratio of 1:1, mixing uniformly, and directly heating and curing in a mould in a programmed way to prepare polyimide; or dissolving in organic solvent, preparing film by tape casting, and heating and drying to obtain polyimide film.
The synthetic route of the preparation method of the invention is as follows:
the preparation of the phosphine benzocyclobutene in the step (1) needs to be carried out in a low-temperature reactor. The anhydrous anaerobic reagent in the step (1) is tetrahydrofuran.
The oxidant in the step (1) is hydrogen peroxide.
The anhydrous reagent in the step (1) is acetone.
The heat curing in the step (2) is performed according to the procedures of 160 ℃/2h,180 ℃/2h,240 ℃/2h,270 ℃/3h,300 ℃/1h and the heating rate of 5 ℃/min.
The organic solvent in the step (2) is N-methylpyrrolidone, dimethylacetamide or dimethylformamide.
The invention is based on the Diels-Alder reaction addition of benzocyclobutene groups in the phosphine oxide benzocyclobutene and carbon-carbon in bismaleimide groups to form a six-membered ring structure, thereby forming the polyimide material. In the reaction process, only heating is needed, no catalyst is needed, no small molecules are generated, and the method is environment-friendly. The prepared phosphine oxide polyimide is an intrinsic high-dielectric polymer material and has excellent thermal stability, and the phosphine has certain flame retardant property. The phosphine oxide polyimide with intrinsic high dielectric property prepared by the invention is expected to be widely applied in the high molecular field.
Drawings
FIG. 1 is a nuclear magnetic resonance spectrum of a phosphonoxybenzocyclobutene (BDPPO) prepared in example 1 of the present invention.
FIG. 2 is a TGA graph of an intrinsic high dielectric property phosphinic polyimide prepared according to the present invention. FIG. 3 is a graph of the dielectric constant of the intrinsic high dielectric properties phosphinic polyimide prepared according to the present invention.
FIG. 4 is a dielectric loss diagram of the intrinsic high dielectric quality phosphinic polyimide prepared according to the present invention.
Having an embodiment of
The following provides representative embodiments of the invention, which are exemplary only and not intended to limit the scope of the invention herein, which are merely illustrative of the methods of practicing the invention:
EXAMPLE 1 Synthesis of the present invention Phosphonobenzocyclobutene (BDPPO)
Into a 500ml round bottom flask were charged 200ml anhydrous anaerobic tetrahydrofuran, 26.54g (0.145 mol) 4-bromobenzocyclobutene and 100ml (0.16 mol) N-butyllithium solution, N 2 Stirring was carried out at-80℃for 2h in an atmosphere. 12.53g (70 mmol) of phenyl phosphorus dichloride are added and stirring is continued for 4h. Standing to room temperature, and steaming to obtain brown phosphine benzocyclobutene.
The obtained benzocyclobutene phosphine was dissolved in 250ml of acetone, stirred well in an ice-water bath, and 20g (0.18 mol) of 30% hydrogen peroxide solution was slowly added dropwise thereto and stirred for 6 hours. Rotary evaporation and drying to obtain white solid, and petroleum ether: ethyl acetate = 10: the 1-chromatography purification can obtain 19.56g of phosphinobenzocyclobutene with the yield of 84.7 percent.
As shown in fig. 1, the nuclear magnetic hydrogen spectrogram of the present invention is analyzed as follows: 1H NMR of BDPPO (400 MHz, CDCl3, delta, ppm): 7.72-7.67 (d, 2H), 7.66-7.64 (s, 1H), 7.58-7.50 (q, 2H), 7.49-7.44 (q, 2H), 7.30-7.36 (d, 2H), 7.17-7.10 (d, 2H), 3.30-3.10 (d, 8H).
The structure of the phosphine oxide Benzocyclobutene (BDPPO) is as follows:
EXAMPLE 2 Synthesis of the inventive Phosphonoxypolyimide with intrinsic high dielectric Properties 1
The mass ratio of the weighed substances is 1:1 the phosphinobenzene 165mg prepared in example 1 and bismaleimide BMI-HC 179mg were mixed well in a flat bottom glass tube 15mm in diameter. At N 2 Under the atmosphere, the cake-shaped polyimide (PI-HC) is obtained by thermal curing according to the procedures of 160 ℃/2h,180 ℃/2h,240 ℃/2h,270 ℃/3h,300 ℃/1h and the temperature rising rate of 5 ℃/min.
The polyimide (PI-HC) has the following structure:
the polyimide (PI-HC) prepared was characterized for thermal properties, wherein the 5% weight loss temperature was 436 ℃, the 10% weight loss temperature was 446 ℃, and the 800 ℃ residual carbon content was 56%.
The prepared polyimide (PI-HC) has dielectric property characterization, dielectric constant of 20.56 and dielectric loss of 0.32. As can be seen from FIG. 3, the dielectric loss of the invention is small, and the material does not generate heat or age.
EXAMPLE 3 Synthesis of the inventive Phosphonoxypolyimide with intrinsic high dielectric Properties 2
The mass ratio of the weighed substances is 1:1 the phosphinobenzene 165mg prepared in example 1 and bismaleimide BMI-12 221mg were mixed well in a flat bottom glass tube 15mm in diameter. At N 2 Under the atmosphere, the program heat is carried out according to 160 ℃/2h,180 ℃/2h,240 ℃/2h,270 ℃/3h,300 ℃/1h and the heating rate is 5 ℃/minSolidifying to obtain cake-shaped polyimide (PI-12).
The polyimide (PI-12) has the following structure:
the polyimide (PI-12) prepared was characterized for thermal properties, wherein the 5% weight loss temperature was 466 ℃, the 10% weight loss temperature was 473 ℃, and the 800 ℃ residual carbon content was 33%.
The prepared polyimide (PI-12) was characterized in terms of dielectric properties, and had a dielectric constant of 14.25 and a dielectric loss of 0.40.
EXAMPLE 4 Synthesis of the inventive Phosphonoxypolyimide with intrinsic high dielectric Properties 3
The mass ratio of the weighed substances is 1: 165mg of the phosphinobenzene prepared in example 1 of 1 and 235mg of bismaleimide BMI-2B were mixed well in a flat bottom glass tube having a diameter of 15 mm. At N 2 Under the atmosphere, the cake-shaped massive polyimide (PI-2B) is obtained by thermal curing according to the procedures of 160 ℃/2h,180 ℃/2h,240 ℃/2h,270 ℃/3h,300 ℃/1h and the temperature rising rate of 5 ℃/min.
The polyimide (PI-2B) has the following structure:
the polyimide (PI-2B) prepared was characterized for thermal properties, wherein the 5% weight loss temperature was 477 ℃, the 10% weight loss temperature was 488 ℃, and the 800 ℃ residual carbon content was 33%.
The prepared polyimide (PI-2B) was characterized for dielectric properties, and had a dielectric constant of 15.06 and a dielectric loss of 0.43.
EXAMPLE 5 Synthesis of the inventive Phosphonoxypolyimide with intrinsic high dielectric Properties 4
The mass ratio of the weighed substances is 1:1 the phosphinobenzocyclobutene 132mg and bismaleimide BMI-80 228mg prepared in example 1 were uniformly mixed in a flat bottom glass tube having a diameter of 15 mm. At N 2 Pressing under atmosphereAnd (3) performing thermal curing by using a program with a temperature rise rate of 5 ℃ per minute at 160 ℃ per 2 hours, 180 ℃ per 2 hours, 240 ℃ per 2 hours, 270 ℃ per 3 hours, 300 ℃ per 1 hour to obtain the cake-shaped massive polyimide (PI-80).
The polyimide (PI-80) has the following structure:
the polyimide (PI-80) prepared was characterized for thermal properties, wherein the 5% weight loss temperature was 427 ℃, the 10% weight loss temperature was 442 ℃, and the 800 ℃ residual carbon content was 46%.
The prepared polyimide (PI-80) is characterized by dielectric property, dielectric constant is 22.56, and dielectric loss is 0.32.
Claims (8)
1. The intrinsic high-dielectric-property phosphinic polyimide has a chemical structural general formula as follows:
wherein n is a positive integer greater than 1.
2. The intrinsic type high dielectric property phosphinic polyimide according to claim 1, wherein R is:
3. the intrinsic type high dielectric property phosphinic polyimide according to claim 1, wherein n is 10000.
4. The process for preparing the intrinsic high dielectric property phosphinic polyimide according to claim 1, which comprises the following synthetic routes:
5. the method for preparing the intrinsic type high dielectric property phosphinic polyimide according to claim 4, which comprises the following steps:
(1) Preparing a monomer: firstly, adding 4-bromobenzocyclobutene and N-butyllithium, N into anhydrous anaerobic reagent 2 Under the condition of-80 ℃ for reaction, adding phenyl dichlorophosphorus for reaction to obtain phosphine benzocyclobutene; in anhydrous reagent, adding oxidant to phosphorus benzocyclobutene to react, and purifying by chromatography with mixed solvent of petroleum ether and ethyl acetate to obtain the phosphine oxide benzocyclobutene.
(2) And (3) a heat curing stage: uniformly mixing the phosphorus oxide benzocyclobutene prepared in the step (1) and bismaleimide, directly heating and solidifying in a die in a program to prepare polyimide or dissolving in an organic solvent, preparing a film by using a tape casting method, and heating and drying in a program to prepare the polyimide film.
6. The method for preparing the intrinsic type high-dielectric-property phosphinic polyimide according to claim 5, which is characterized in that: petroleum ether in the mixed solvent of petroleum ether and ethyl acetate in the step (1): the volume ratio of the ethyl acetate is 10:1.
7. the method for preparing the intrinsic type high-dielectric-property phosphinic polyimide according to claim 5, which is characterized in that: the anhydrous anaerobic reagent in the step (1) is tetrahydrofuran; the oxidant is hydrogen peroxide; the anhydrous reagent is acetone.
8. The method for preparing the intrinsic type high-dielectric-property phosphinic polyimide according to claim 5, which is characterized in that: the heat curing in the step (2) is performed according to the procedures of 160 ℃/2h,180 ℃/2h,240 ℃/2h,270 ℃/3h,300 ℃/1h and the heating rate of 5 ℃/min; the organic solvent in the step (2) is N-methylpyrrolidone, dimethylacetamide or dimethylformamide.
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