CN109679095A - A kind of high temperature resistant type polyamide-polyether acid imide toughening polymer and preparation method thereof - Google Patents
A kind of high temperature resistant type polyamide-polyether acid imide toughening polymer and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a kind of high temperature resistant type polyamide-polyether acid imide toughening polymer, the strand of the polymer toughening micro mist includes the constitutional repeating unit as shown in formula (I), formula (II) and formula (III).The invention also discloses the preparation method of above-mentioned high temperature resistant type polyamide-polyether acid imide toughening micro mist, the high temperature resistant type polyamide-polyether acid imide toughening micro mist that the present invention is prepared has the characteristics that high heat resistance and high tenacity, has broad application prospects.
Description
Technical field
The invention belongs to technical field of polymer materials, and in particular to a kind of high temperature resistant type polyamide-polyether acid imide increasing
Tough micro mist and preparation method thereof.
Background technique
Fiber reinforcement thermosetting matrix resin composite material, such as carbon fiber-cyanate ester resin composite material, because of its specific strength
It is prominent with the performance of specific modulus etc. and obtain a large amount of application in high structural strength & lightweight demand side；But it is this
Thermoset substrate resin generally comprises the thermoplastic particles of one or more of " toughenings ", such as polyetherimide superfine powder and polyamides
Amine-acid imide superfine powder.The polyetherimide superfine powder of " toughening " that has been commercialized, such as the polyetherimide of Sabic company, Saudi Arabia
Amine superfine powder Ultem 1000F3SP, the simply supported beam unnotched impact strength for representing its toughness are higher by no toughening cyanate ester resin and consolidate
Compound several times, still, represent its can long-term use temperature heat distortion temperature (HDT, 1.82MPa) only at 200 DEG C hereinafter, heatproof
Grade is lower；The polyamide-imides superfine powder of " toughening " that has been commercialized, such as Torlon of Solvay company, Belgium
4000TF, although represent can long-term use temperature heat distortion temperature (HDT, 1.82MPa) at 240 DEG C or more, temperature resistant grade compared with
Height, still, the simply supported beam unnotched impact strength for representing its toughness are more much lower than polyetherimide superfine powder.Reinforcedathermoset matrices
Resin, at 230 DEG C the long-term use temperature after solidifying such as cyanate matrix resin or Bmi In Fiber Composites etc.
More than, so, while using polyetherimide superfine powder and polyamide-imides superfine powder as such matrix resin " toughening "
Thermoplastic particles can not meet the requirement of high heat resistance and high tenacity simultaneously.
Summary of the invention
The technical problem to be solved in the present invention is to provide a kind of high temperature resistant type polyamide-polyether acid imide toughening particles, make
For the thermoplastic of high temperature resistant thermosetting matrix resin (such as cyanate matrix resin or Bmi In Fiber Composites) " toughening "
Property particle, can meet the requirement of high heat resistance and high tenacity simultaneously.
In order to solve the above technical problems, the present invention adopts the following technical scheme:
A kind of high temperature resistant type polyamide-polyether acid imide toughening polymer it is characterized in that, the polymer strand packet
Include the molecule of the constitutional repeating unit as shown in formula (I), formula (II) and formula (III).
In Formulas I and formula II, X is divalent functional group, and structure is shown in formula (A)~(C) is any:
The structure of X or be 4,4 '-diaminobenzene Formanilides, 3,3 '-diaminobenzene Formanilides, 3,4 '-two
Aminobenzoic anilid, 4,3 '-diaminobenzene Formanilides；Bis- (the 4- aminobenzoyl replaces) phenylenediamines of Isosorbide-5-Nitrae-, Isosorbide-5-Nitrae-are bis-
(3- aminobenzoyl replaces) phenylenediamine, 1- (4- aminobenzoyl replaces) -4- (3- aminobenzoyl replaces) phenylenediamine；Bis- (the 4- of 1,3-
Aminobenzoyl replaces) phenylenediamine, 1,3- bis- (3- aminobenzoyl replaces) phenylenediamines, 1- (4- aminobenzoyl replaces) -3- (3- amino
Benzoyl replaces) phenylenediamine；(Isosorbide-5-Nitrae-phenyl-diformyl replaces) is bis- (4- amino aniline), (Isosorbide-5-Nitrae-phenyl-diformyl replaces) bis- (3- aminobenzenes
Amine), Isosorbide-5-Nitrae-phenyl-diformyl replaces [(4- amino aniline), (3- amino aniline)]；(1,3- phenyl-diformyl replaces) is bis- (4- amino aniline),
(1,3- phenyl-diformyl replaces) bis- (3- amino anilines) or 1,3- phenyl-diformyl are in [(4- amino aniline), (3- amino aniline)]
Any one；
In formula III, Y is tetravalence functional group, and structure is shown in formula (D)~(I) is any:
The structure of Y or be 1,2,4,5- pyromellitic acid anhydride, 3,3 ', 4,4 '-bibenzene tetracarboxylic dianhydrides, 3,3 ', 4,
4 '-diphenyl ether tetraformic dianhydrides, 3,3 ', 4,4 '-benzophenone tetracarboxylic dianhydrides, 4,4 '-(4,4 '-isopropyl diphenoxies) are double
Any one in (phthalic anhydride) or 4,4 '-(4,4 '-hexafluoro isopropyl, two phenoxy group) bis- (phthalic anhydrides).
In formula III, Z is divalent functional group, shown in structure such as formula (J)~formula (S):
Wherein, R1It is-OH ,-COOH or-OCOR3Substituent group；R2It is-H ,-OH ,-COOH ,-OCOR3Substituent group；R3It is monovalence
Alkane or monovalence aromatic hydrocarbons substituent group；
In Formulas I, formula II and formula III, l, m and n are 0 or natural number, but l and m cannot be 0 simultaneously；Moreover, Formulas I, II and of formula
L, m and n in formula III must simultaneously meet following conditions: (l+m)/(l+m+n) >=0.6,
Wherein, Z are as follows: 3,5- diaminobenzoic acids, 3,5- diaminophenol, the carboxylic acid esters of 3,5- diaminophenol are derivative
Object, 4,6- diaminostilbene, 3- dihydroxy benzenes, 4,6- diaminostilbene, the ramification of carboxylic esters of 3- dihydroxy benzenes, 3,3 '-diaminos
Base -4,4 '-dihydroxybiphenyl, the ramification of carboxylic esters of 3,3 '--4,4 '-dihydroxybiphenyls of diamino, 4,4 '-diamino -3,
Bis- (3- amino -4- the hydroxyls of ramification of carboxylic esters, 2,2- of 3 '-dihydroxybiphenyls, 4,4 '--3,3 '-dihydroxybiphenyls of diamino
Base phenyl) propane, bis- (3- amino-4-hydroxylphenyl) propane of 2,2- the bis- (3- amino -4- hydroxyls of ramification of carboxylic esters, 2,2-
Base phenyl) hexafluoropropane or bis- (3- amino-4-hydroxylphenyl) hexafluoropropane of 2,2- ramification of carboxylic esters.
Wherein, X and Z is identical structure or different structure.
The preparation method of above-mentioned high temperature resistant type polyamide-polyether acid imide toughening micro mist, includes the following steps:
(1) in polar non-solute, it is firstly added diamines, stirring and dissolving is complete at 25~50 DEG C, solution temperature
It is preferred that 35 DEG C；It is cooled to 10~20 DEG C, preferably 15 DEG C again, is added dianhydride, the molar ratio of dianhydride and diamines is 0.99~1.01, is stirred
It mixes polymerization 10~15 hours, generates polyamic acid resin；
(2) mixture of 0.2~0.55 times of solvent volume amount toluene, dimethylbenzene or both is added, then is rapidly heated back
Stream band water 12~24 hours, finally distillation is warming up to polar non-solute boiling point, isolates toluene, dimethylbenzene or theirs is mixed
Object is closed, polyamide-polyether acid imide turbid solution is obtained；In the polyamide-polyether acid imide turbid solution preparation process, solid content
Mass fraction is gross mass/(gross mass of solvent quality+dianhydride and diamines) of dianhydride and diamines 5~45%, preferably 15%
It is exactly polyamic acid solid content, that is, the mass fraction of polyamic acid solid content.
(3) solid quality of polyamide-polyether acid imide turbid solution is adjusted with the polar non-solute in step (1)
Fractional content is 5~20%, is spray-dried on drying machine with centrifugal spray, obtains polyamide-polyether acid imide toughening micro mist.
In step (1), the polar non-solute is N-Methyl pyrrolidone, dimethyl sulfoxide, N, N- dimethyl second
The mixture of one or more of amide, n,N-Dimethylformamide, preferably N-Methyl pyrrolidone.
In step (1), the diamines is 4,4 '-diaminobenzene Formanilides, bis- (the 3- amino-4-hydroxy benzene of 2,2-
Base) propane；(1,4- phenyl-diformyl replaces) bis- (4- amino anilines), bis- (3- amino-4-hydroxylphenyl) hexafluoropropane of 2,2-；1,3-
One or more of mixture in bis- (the 4- aminobenzoyl replaces) phenylenediamines of bis- (4- aminobenzoyl replaces) phenylenediamines, 1,4-.
In step (1), the dianhydride is 4,4 '-(4,4 '-isopropyl diphenoxy) bis- (phthalic anhydrides), 4,
One in 4 '-(4,4 '-hexafluoro isopropyl, two phenoxy group) bis- (phthalic anhydrides), 3,3 ', 4,4 '-benzophenone tetracarboxylic dianhydrides
Kind or several mixtures.
In step (3), the drying condition of the spray drying are as follows: 195~260 DEG C of inlet air temperature；Leaving air temp 90~140
℃；Spray amount is 5~50Kg/hr.
Beneficial effect
The invention discloses a kind of polyamide-polyether acid imide toughening micro mists, have the feature that
1) specific particle size distribution characteristic: D (05)≤1 μm, D (50)≤35 μm, (95)≤75 μm D；
2) simply supported beam unnotched impact strength >=160KJ/m2；
3) heat distortion temperature (HDT, 1.82MPa) is at 250 DEG C or more；
4) Te Nian Du≤0.43dL/g；
Polyamide-polyether acid imide toughening micro mist prepared by the present invention can meet the requirement of high heat resistance and high tenacity simultaneously,
It has broad application prospects.
Specific embodiment
Polyamide-polyether acid imide turbid solution preparation process is as follows:
In polar non-solute (such as N-Methyl pyrrolidone, dimethyl sulfoxide, DMAC N,N' dimethyl acetamide, N, N- bis-
Methylformamide etc. or they arbitrarily arrange in pairs or groups the mixed solvent of arbitrary proportion) in, be firstly added diamines, stirred at 25~50 DEG C
Dissolution is complete；It is cooled between 10~20 DEG C again, dianhydride is added, stirring polymerization 10~15 hours generates polyamic acid resin；Add
Enter 0.2~0.55 times of quantity of solvent of toluene, dimethylbenzene or their mixture, then be rapidly heated reflux band water 12~24 hours,
Distillation is warming up to polar non-solute boiling point later, isolates toluene, dimethylbenzene or their mixture, obtains polyamide-
Polyetherimide turbid solution.In the polyamide-polyether acid imide turbid solution preparation process, select solid content in 5~45% (Wt.)
Between.
Dirty solution spray-drying process is with identical solvent by the solid content tune of above-mentioned polyamide-polyether acid imide turbid solution
It is whole between 5~20%, it is dry that Direct spraying is carried out on the type drying machine with centrifugal spray of LPG-5~50；Hothouse inlet air temperature
Between 195~260 DEG C, 90~140 DEG C of leaving air temp, spray amount is between 5~50Kg/hr.Powder is collected, is exactly the polyamides
Amine-polyetherimide toughening micro mist.
Sample test reference standard is as follows in the present invention:
1, laser particle size measurement: according to the wet process in examination criteria GB/T 19077.1-2003 to the polyimides toughening
Fine grain final product carries out testing graininess.
2, simply supported beam unnotched impact strength: according to examination criteria GB/T 1043.1-2008, by all test sample systems
At the test bars of predetermined size, simply supported beam unnotched impact strength is tested.
3, heat distortion temperature: sample is carried out using 1.82MPa load according to examination criteria GB/T 1634.1-2004
Heat distortion temperature detection.
4, inherent viscosity: according to examination criteria GB/T 1632.5-2008, solvent is made using NMP, selects Φ 0.84mm's
Ubbelohde viscosity tube carries out inherent viscosity detection to sample.
Embodiment 1:
Polyamide-polyether acid imide turbid solution preparation process is firstly added in 878.96 grams of N-Methyl pyrrolidones
36.362 gram 4,4 '-diaminobenzene Formanilides and bis- (3- amino-4-hydroxylphenyl) propane of 10.333 grams of 2,2-, 25~
Stirring and dissolving is complete at 50 DEG C；It is cooled between 10~20 DEG C again, is added 83.278 gram 4,4 '-(4,4 '-isopropyl diphenyl oxygen
Base) bis- (phthalic anhydrides) and 25.137 gram 4,4 '-(4,4 '-hexafluoro isopropyl, two phenoxy group) bis- (phthalic anhydrides),
Stirring polymerization 14 hours, generates polyamic acid resin；439.48 grams of toluene are added, then are rapidly heated reflux band water 22 hours, most
Distillation is warming up to N-Methyl pyrrolidone boiling point and stops steaming afterwards, isolates 512.62 grams of toluene fraction, adds into reaction system
73.14 grams of N-Methyl pyrrolidones make system solid content be maintained at 15% (Wt.).It is muddy to obtain polyamide-polyether acid imide
Liquid.
Dirty solution spray-drying process is with identical solvent by the solid content tune of above-mentioned polyamide-polyether acid imide turbid solution
It is whole between 15%, it is dry that Direct spraying is carried out on LPG-15 type drying machine with centrifugal spray；250 DEG C of hothouse inlet air temperature,
Between 135 DEG C of leaving air temp, spray amount is between 12Kg/hr.Powder is collected, is exactly that the polyamide-polyether acid imide toughening is micro-
Powder.
Sample carries out performance detection or test according to aforementioned examination criteria.
Embodiment 2:
In addition to formula, the preparation process with embodiment 1 of polyamide-polyether acid imide toughening particle is complete in the present embodiment
It is identical.The formula of the present embodiment is as follows: 952.36 grams of N-Methyl pyrrolidones, and 36.362 gram 4,4 '-diaminobenzene formyls replace benzene
Amine and bis- (3- amino-4-hydroxylphenyl) propane of 10.333 grams of 2,2-, 20.820 gram 4,4 '-(4,4 '-isopropyl diphenoxies)
Bis- (phthalic anhydrides) and 100.549 gram 4,4 '-(4,4 '-hexafluoro isopropyl, two phenoxy group) bis- (phthalic anhydrides).It returns
476.18 grams of toluene are added before stream, isolates 559.76 grams of toluene fraction, adds 83.58 grams of N-Methyl pyrrolidones.
Sample carries out performance detection or test according to aforementioned examination criteria.
Embodiment 3:
In addition to formula, the preparation process with embodiment 1 of polyamide-polyether acid imide toughening particle is complete in the present embodiment
It is identical.The formula of the present embodiment is as follows: 911.69 grams of N-Methyl pyrrolidones, 45.029 grams of (Isosorbide-5-Nitrae-phenyl-diformyl replaces) bis- (4-
Amino aniline) and bis- (3- amino-4-hydroxylphenyl) hexafluoropropane of 25.638 grams of 2,2-, 67.664 gram 4,4 '-(4,4 '-isopropyls
Two phenoxy group of base) bis- (phthalic anhydrides) and 22.555 gram of 3,3 ', 4,4 '-benzophenone tetracarboxylic dianhydride.It is added before reflux
455.84 grams of toluene isolate 535.85 grams of toluene fraction, add 80.01 grams of N-Methyl pyrrolidones.
Sample carries out performance detection or test according to aforementioned examination criteria.
Embodiment 4:
In addition to formula, the preparation process with embodiment 1 of polyamide-polyether acid imide toughening particle is complete in the present embodiment
It is identical.The formula of the present embodiment is as follows: 982.45 grams of N-Methyl pyrrolidones, 69.276 grams of 1,3- bis- (4- aminobenzoyl replaces)
Phenylenediamine, 104.098 gram 4,4 '-(4,4 '-isopropyl diphenoxy) bis- (phthalic anhydrides).491.23 grams are added before reflux
Toluene isolates 577.45 grams of toluene fraction, adds 86.22 grams of N-Methyl pyrrolidones.
Sample carries out performance detection or test according to aforementioned examination criteria.
Embodiment 5:
In addition to formula, the preparation process with embodiment 1 of polyamide-polyether acid imide toughening particle is complete in the present embodiment
It is identical.The formula of the present embodiment is as follows: 828.59 grams of N-Methyl pyrrolidones, and 51.957 grams of Isosorbide-5-Nitraes-are bis- (4- aminobenzoyl replaces)
Phenylenediamine, 94.265 gram 4,4 '-(4,4 '-hexafluoro isopropyl, two phenoxy group) bis- (phthalic anhydrides).It is added before reflux
414.30 grams of toluene isolate 487.02 grams of toluene fraction, add 72.72 grams of N-Methyl pyrrolidones.
Sample carries out performance detection or test according to aforementioned examination criteria.
In the invention patent, select the polyamide-imides superfine powder (such as Torlon 4000TF) being commercialized as
The sample of comparative example 1, selecting the polyetherimide superfine powder (such as ULTEM 1000F3SP) as a comparison case 2 being commercialized
Sample.Sample carries out performance detection or test also according to aforementioned examination criteria.
The properties of sample of all embodiment and comparative examples detects or test result is as described in Table 1.
From table 1 it follows that polyamide-polyether acid imide toughening particle, temperature resistant grade provided by the invention patent
It is all higher with toughness, " increase as thermoset substrate resin (such as cyanate matrix resin or Bmi In Fiber Composites)
It is tough " thermoplastic particles, have and meet the more preferable performance basis of high heat resistance and high tenacity.
1 sample detection result of table
Claims (8)
1. a kind of high temperature resistant type polyamide-polyether acid imide toughening polymer, which is characterized in that the strand of the polymer includes
The constitutional repeating unit as shown in formula (I), formula (II) and formula (III).
In Formulas I and formula II, X is divalent functional groups, and structure is shown in formula (A)~(C) is any:
The structure of X is 4,4 '-diaminobenzene Formanilides, 3,3 '-diaminobenzene Formanilides, 3,4 '-diamino
Benzoyl replaces aniline, 4,3 '-diaminobenzene Formanilides, bis- (the 4- aminobenzoyl replaces) phenylenediamines of 1,4-, bis- (the 3- ammonia of 1,4-
Base benzoyl replaces) phenylenediamine, 1- (4- aminobenzoyl replaces) -4- (3- aminobenzoyl replaces) phenylenediamine, bis- (the 4- aminobenzenes of 1,3-
Formyl replaces) phenylenediamine, bis- (the 3- aminobenzoyl replaces) phenylenediamines of 1,3-, 1- (4- aminobenzoyl replaces) -3- (3- aminobenzoyl
For) phenylenediamine, (1,4- phenyl-diformyl replaces) bis- (4- amino anilines), (1,4- phenyl-diformyl replaces) bis- (3- amino anilines), 1,4-
Phenyl-diformyl replaces [(4- amino aniline), (3- amino aniline)], (1,3- phenyl-diformyl replaces) bis- (4- amino anilines), (1,3- benzene
Two formyls replace) bis- (3- amino anilines), 1,3- phenyl-diformyl is for any one in [(4- amino aniline), (3- amino aniline)]
Kind；
In formula III, Y is tetravalence functional group, and structure is shown in formula (D)~(I) is any:
The structure of Y is 1,2,4,5- pyromellitic acid anhydride, 3,3 ', 4,4 '-bibenzene tetracarboxylic dianhydrides, 3,3 ', 4,4 '-two
Phenylate tetracarboxylic acid dianhydride, 3,3 ', 4,4 '-benzophenone tetracarboxylic dianhydrides, 4,4 '-(4,4 '-isopropyl diphenoxy) bis- (adjacent benzene
Dicarboxylic acid anhydride) or 4,4 '-(4,4 '-hexafluoro isopropyl, two phenoxy group) bis- (phthalic anhydrides) in any one.
In formula III, Z is divalent functional group, shown in structure such as formula (J)~formula (S):
Wherein, R1It is-OH ,-COOH or-OCOR3Substituent group；R2It is-H ,-OH ,-COOH ,-OCOR3Substituent group；R3It is monovalent alkane
Or monovalence aromatic hydrocarbons substituent group；
In Formulas I, formula II and formula III, l, m and n are 0 or natural number, but l and m cannot be 0 simultaneously；Moreover, Formulas I, formula II and formula III
In l, m and n must simultaneously meet following conditions: (l+m)/(l+m+n) >=0.6,
2. high temperature resistant type polyamide-polyether acid imide toughening polymer according to claim 1, which is characterized in that Z are as follows: 3,
5- diaminobenzoic acid, 3,5- diaminophenol, the ramification of carboxylic esters of 3,5- diaminophenol, 4,6- diaminostilbene, 3-
Dihydroxy benzenes, 4,6- diaminostilbene, the ramification of carboxylic esters of 3- dihydroxy benzenes, 3,3 '--4,4 '-dihydroxybiphenyls of diamino,
The ramification of carboxylic esters of 3,3 '--4,4 '-dihydroxybiphenyls of diamino, 4,4 '-diamino -3,3 '-dihydroxybiphenyl, 4,4 ' -
Bis- (3- amino-4-hydroxylphenyl) propane of diamino -3,3 '-dihydroxybiphenyl ramification of carboxylic esters, 2,2-, 2,2- are bis-
Bis- (3- amino-4-hydroxylphenyl) hexafluoropropane or 2 of the ramification of carboxylic esters, 2,2- of (3- amino-4-hydroxylphenyl) propane,
The ramification of carboxylic esters of bis- (3- amino-4-hydroxylphenyl) hexafluoropropane of 2-.
3. high temperature resistant type polyamide-polyether acid imide toughening polymer according to claim 1, which is characterized in that X and Z are
Identical structure or different structure.
4. the preparation method of any high temperature resistant type polyamide-polyether acid imide toughening polymer of claims 1 to 3, special
Sign is, includes the following steps:
(1) in polar non-solute, it is firstly added diamines, stirring and dissolving is complete at 25~50 DEG C；It is cooled to 10 again~
20 DEG C, dianhydride is added, the molar ratio of dianhydride and diamines is 0.99~1.01, and stirring polymerization 10~15 hours generates polyamic acid
Resin；
(2) mixture of 0.2~0.55 times of solvent volume amount toluene, dimethylbenzene or both, then the band that flows back that is rapidly heated is added
Water 12~24 hours, finally distillation was warming up to polar non-solute boiling point, isolates toluene, dimethylbenzene, and it is poly- to obtain polyamide-
Etherimide turbid solution；In the polyamide-polyether acid imide turbid solution preparation process, the mass fraction of solid content be 5~
45%.
(3) total solid content of polyamide-polyether acid imide turbid solution is adjusted with the polar non-solute in step (1)
Content is 5~20%, is spray-dried on drying machine with centrifugal spray, obtains polyamide-polyether acid imide toughening micro mist.
5. the preparation method of high temperature resistant type polyamide-polyether acid imide toughening polymer, feature exist according to claim 4
In the polar non-solute is N-Methyl pyrrolidone, dimethyl sulfoxide, n,N-dimethylacetamide, N, N- dimethyl
The mixture of one or more of formamide.
6. the preparation method of high temperature resistant type polyamide-polyether acid imide toughening polymer, feature exist according to claim 4
In in step (1), the diamines is 4,4 '-diaminobenzene Formanilides, bis- (the 3- amino-4-hydroxylphenyls) third of 2,2-
Alkane；(1,4- phenyl-diformyl replaces) bis- (4- amino anilines), bis- (3- amino-4-hydroxylphenyl) hexafluoropropane of 2,2-；3,3 '-diaminos
Base benzoyl replaces aniline, bis- (the 4- aminobenzoyl replaces) phenylenediamines of 1,3-, 1,3- bis- (4- aminobenzoyl replaces) phenylenediamines, 1,4-
One or more of mixture in bis- (4- aminobenzoyl replaces) phenylenediamines.
7. the preparation method of high temperature resistant type polyamide-polyether acid imide toughening polymer, feature exist according to claim 4
In, in step (1), the dianhydride be 4,4 '-(4,4 '-isopropyl diphenoxy) bis- (phthalic anhydrides), 4,4 '-(4,
4 '-hexafluoro isopropyl, two phenoxy group) bis- (phthalic anhydrides), 3,3 ', 4,4 '-diphenyl ether tetraformic dianhydrides, 3,3 ', 4,4 '-
One or more of mixture in benzophenone tetracarboxylic dianhydride.
8. the preparation method of high temperature resistant type polyamide-polyether acid imide toughening polymer, feature exist according to claim 4
In, in step (3), the drying condition of the spray drying are as follows: 195~260 DEG C of inlet air temperature, 90~140 DEG C of leaving air temp, spray
Mist amount is 5~50Kg/hr.
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| CN111440336A (en) * | 2020-03-09 | 2020-07-24 | 苏州予信天材新材料应用技术有限公司 | Surface modified polyimide particle and preparation method and application thereof |
| CN112500567A (en) * | 2020-12-21 | 2021-03-16 | 奥克控股集团股份公司 | High-modulus transparent polyimide film material containing amide structure and preparation method thereof |
| TWI799833B (en) * | 2021-04-15 | 2023-04-21 | 達興材料股份有限公司 | Polyimide precursor, resin composition, polyimide, polyimide used for protective sacrificial layer between semiconductor wafer and encapsulation material, and semiconductor element with protective sacrificial layer |
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| CN111440336A (en) * | 2020-03-09 | 2020-07-24 | 苏州予信天材新材料应用技术有限公司 | Surface modified polyimide particle and preparation method and application thereof |
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| CN112500567A (en) * | 2020-12-21 | 2021-03-16 | 奥克控股集团股份公司 | High-modulus transparent polyimide film material containing amide structure and preparation method thereof |
| CN112500567B (en) * | 2020-12-21 | 2023-03-14 | 奥克控股集团股份公司 | High-modulus transparent polyimide film material containing amide structure and preparation method thereof |
| TWI799833B (en) * | 2021-04-15 | 2023-04-21 | 達興材料股份有限公司 | Polyimide precursor, resin composition, polyimide, polyimide used for protective sacrificial layer between semiconductor wafer and encapsulation material, and semiconductor element with protective sacrificial layer |
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| CN114621440A (en) | 2022-06-14 |
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