CN110330791A - A kind of preparation method and product of the Kapton of cold cycling treatment repeatedly - Google Patents
A kind of preparation method and product of the Kapton of cold cycling treatment repeatedly Download PDFInfo
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- CN110330791A CN110330791A CN201910719637.9A CN201910719637A CN110330791A CN 110330791 A CN110330791 A CN 110330791A CN 201910719637 A CN201910719637 A CN 201910719637A CN 110330791 A CN110330791 A CN 110330791A
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- 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
- C08G73/10—Polyimides; Polyester-imides; Polyamide-imides; Polyamide acids or similar polyimide precursors
- C08G73/1003—Preparatory processes
- C08G73/1007—Preparatory processes from tetracarboxylic acids or derivatives and diamines
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- 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
- C08G73/10—Polyimides; Polyester-imides; Polyamide-imides; Polyamide acids or similar polyimide precursors
- C08G73/1039—Polyimides; Polyester-imides; Polyamide-imides; Polyamide acids or similar polyimide precursors comprising halogen-containing substituents
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- 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
- C08G73/10—Polyimides; Polyester-imides; Polyamide-imides; Polyamide acids or similar polyimide precursors
- C08G73/1057—Polyimides containing other atoms than carbon, hydrogen, nitrogen or oxygen in the main chain
- C08G73/1064—Polyimides containing other atoms than carbon, hydrogen, nitrogen or oxygen in the main chain containing sulfur
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- 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
- C08G73/10—Polyimides; Polyester-imides; Polyamide-imides; Polyamide acids or similar polyimide precursors
- C08G73/1067—Wholly aromatic polyimides, i.e. having both tetracarboxylic and diamino moieties aromatically bound
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J5/00—Manufacture of articles or shaped materials containing macromolecular substances
- C08J5/18—Manufacture of films or sheets
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2379/00—Characterised by the use of macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing nitrogen with or without oxygen, or carbon only, not provided for in groups C08J2361/00 - C08J2377/00
- C08J2379/04—Polycondensates having nitrogen-containing heterocyclic rings in the main chain; Polyhydrazides; Polyamide acids or similar polyimide precursors
- C08J2379/08—Polyimides; Polyester-imides; Polyamide-imides; Polyamide acids or similar polyimide precursors
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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
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/38—Boron-containing compounds
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Abstract
The invention discloses the preparation methods and product of a kind of cold cycling treatment Kapton repeatedly, are made of the raw material of following parts by weight: 1000-1500 parts of diamines, 1000-1500 parts of dianhydride, 10-20 parts of catalyst, 30-50 parts of paigeite.The operation of cold cycling treatment is introduced repeatedly in imidization, and is added to paigeite, considerably increases the fracture resistance and alkali corrosion resistance performance of Kapton, improves performance of the material in flexible circuit application.
Description
Technical field
The invention belongs to imide membrane preparation technical fields, and in particular to a kind of cold cycling treatment polyimides repeatedly
The preparation method and product of film.
Background technique
Polyimides is a kind of with high-modulus, the engineering plastics of low water absorption and resistance to thermo oxidative stability.Currently, polyamides
Imines has increasingly received the attention and exploitation of people.It is taken the lead by former Machinery Ministry and the Ministry of Chemical Industry in the seventies, researches and develops this in China
Kind material, is used for electric insulation.With China's digital product, intelligent appliance, the fast development of automotive electronics etc. has pushed flexibility
The rapid growth in circuit board market.Such as Mobile Industry, 1 conventional mobile phone demand about 2-3 piece flexible circuit board, high-grade mobile phone
5-6 piece, smart phone are then 6-8 pieces.The Kapton demand in China flexible circuit field is up to 5000 tons, and year by year
It is incremented by, China's Kapton product scale is annual up to 4700 tons, but most of product low side, is mainly used in insulating materials
85% or more the Kapton in field, the application of flexible circuit field relies on import.
Flexible circuit needs material to have stronger folding and corrosion resistance, the current polyimides for making flexible circuit
Material, although flexibility is done well, generally existing folding quality is poor, the problem of alkali resistance substance corrosive nature difference.
Summary of the invention
The purpose of the present invention is to provide the preparation methods and product of a kind of cold cycling treatment Kapton repeatedly.
A kind of cold cycling treatment Kapton repeatedly, is made: diamines 1000- of the raw material of following parts by weight
1500 parts, 1000-1500 parts of dianhydride, 10-20 parts of catalyst, 30-50 parts of paigeite.
Paigeite belongs to boric acid salt mine, orthorhombic system, (Mg, Fe2+)2Fe(3+)[BO3]O2, cell parameter, A0:9.37, B0:
3.05, C0:12.36, α: 0, β: 0, γ: 0；Containing a little unknown impuritie.Paigeite is industrially the raw material for refining borax, China
Resource reserve is abundant, and paigeite is added in inventor's discovery in Kapton preparation process, then cold cycling treatment repeatedly,
The fracture resistance of material can be significantly increased, the substance in paigeite is mostly the crystal of iron and boron oxide compound, and chemical property is very
Stablize, cannot be chemically reacted with highly basic, thus has been significantly enhanced the alkaline resistance properties of material.
The diamines be 3,3 '-dimethylbenzidines, 4,4 '-diaminobenzophenones, 2,4- diamino -6- chlorotoluenes,
2,2'- bis- [4- (4- amino-benzene oxygen) phenyl] hexafluoropropane, 2,2'- bis- [4- (4- amino-benzene oxygen) phenyl] propane or Isosorbide-5-Nitrae-
Bis- (4- amino-benzene oxygen) benzene.
The dianhydride is 3,3 ', 4,4 '-biphenyltetracarboxylic dianhydrides, Isosorbide-5-Nitrae, 5,8- naphthalene tetracarboxylic acid dianhydrides, phenanthrene -1,8,9,10-
Tetracarboxylic dianhydride, 3,4,3', 4'- diphenyl ether dianhydride or 2,3,3', 4'- diphenyl ether dianhydride.
The catalyst is triethylamine, N, N- dimethyl cyclohexyl amine, N, N- dimethyl benzylamine, triethanolamine, N, N- diformazan
Ethylethanolamine or isoquinolin.
A kind of preparation method of the Kapton of cold cycling treatment repeatedly carries out in accordance with the following steps:
(1) diamines and dianhydride are mixed, catalyst are added, be heated to 50-100 DEG C of initiated polymerization, stir 12-36h,
Slurry is made；
(2) paigeite is crushed, is milled, cross 100-160 mesh, be put into the slurry of step (1) preparation, stir evenly,
Coating liquid is made；
(3) coating liquid by step (2) preparation is sent into extrusion coating machine, and coating liquid is applied to steel band by extrusion die
On, the thickness of film is controlled by the gap of electronic control pressing die head outlet；
(4) polyimide film by step (3) by extrusion coated film forming is sent into imidization furnace, carries out imidization processing,
Finally by cold cycling treatment repeatedly, final products are obtained.
The time interval of the cold cycling treatment repeatedly is 10-15s, and SAPMAC method temperature is 40-45 DEG C, thermal cycling temperature
It is 160-170 DEG C, cycle-index is 40-60 times.
Beneficial effects of the present invention: Kapton prepared by the present invention, using cold cycling repeatedly in preparation process
Processing, and it is added to paigeite, the fracture resistance and alkali corrosion resistance performance of Kapton are considerably increased, material is improved
Expect the performance in flexible circuit application.
Specific embodiment
The present invention will be further described combined with specific embodiments below.
Embodiment 1
A kind of cold cycling treatment Kapton repeatedly, is made: 3,3 '-dimethyl of the raw material of following parts by weight
1300 parts of benzidine, 3,3 ', 4,4 ' -1300 parts of biphenyltetracarboxylic dianhydrides, 15 parts of triethylamine, 40 parts of paigeite.
The preparation method of the above-mentioned Kapton of cold cycling treatment repeatedly carries out in accordance with the following steps:
(1) by 3,3 '-dimethylbenzidines and 3, triethylamine, heating is added in the mixing of 3 ', 4,4 '-biphenyltetracarboxylic dianhydrides
To 80 DEG C of initiated polymerizations, for 24 hours, slurry is made in stirring；
(2) paigeite is crushed, is milled, cross 120 meshes, be put into the slurry of step (1) preparation, stir evenly, be made
Coating liquid；
(3) coating liquid by step (2) preparation is sent into extrusion coating machine, and coating liquid is applied to steel band by extrusion die
On, the thickness of film is controlled by the gap of electronic control pressing die head outlet；
(4) polyimide film by step (3) by extrusion coated film forming is sent into imidization furnace, carries out imidization processing,
Finally by cold cycling treatment repeatedly, final products are obtained；The time interval of the cold cycling treatment repeatedly is 12s, cold
Circulating temperature is 42 DEG C, and thermal cycling temperature is 165 DEG C, and cycle-index is 50 times.
Embodiment 2
A kind of cold cycling treatment Kapton repeatedly, is made: 4,4 '-diamino of the raw material of following parts by weight
1000 parts of benzophenone, Isosorbide-5-Nitrae, 5,8- 1000 parts of naphthalene tetracarboxylic acid dianhydrides, N, 12 parts of N- dimethyl cyclohexyl amine, 32 parts of paigeite.
The preparation method of the above-mentioned Kapton of cold cycling treatment repeatedly carries out in accordance with the following steps:
(1) diamines and dianhydride are mixed, catalyst is added, be heated to 70 DEG C of initiated polymerizations, stir 36h, slurry is made
Material；
(2) paigeite is crushed, is milled, cross 150 meshes, be put into the slurry of step (1) preparation, stir evenly, be made
Coating liquid；
(3) coating liquid by step (2) preparation is sent into extrusion coating machine, and coating liquid is applied to steel band by extrusion die
On, the thickness of film is controlled by the gap of electronic control pressing die head outlet；
(4) polyimide film by step (3) by extrusion coated film forming is sent into imidization furnace, carries out imidization processing,
Finally by cold cycling treatment repeatedly, final products are obtained；The time interval of the cold cycling treatment repeatedly is 10s, cold
Circulating temperature is 40 DEG C, and thermal cycling temperature is 160 DEG C, and cycle-index is 40 times.
Embodiment 3
A kind of cold cycling treatment Kapton repeatedly, is made: 2,4- diamino-of the raw material of following parts by weight
1400 parts of 6- chlorotoluene, 1400 parts of tetracarboxylic dianhydride, N, 18 parts of N- dimethyl benzylamine, 45 parts of paigeite of phenanthrene -1,8,9,10-.
The preparation method of the above-mentioned Kapton of cold cycling treatment repeatedly carries out in accordance with the following steps:
(1) diamines and dianhydride are mixed, catalyst is added, be heated to 90 DEG C of initiated polymerizations, stir 18h, slurry is made
Material；
(2) paigeite is crushed, is milled, cross 120 meshes, be put into the slurry of step (1) preparation, stir evenly, be made
Coating liquid；
(3) coating liquid by step (2) preparation is sent into extrusion coating machine, and coating liquid is applied to steel band by extrusion die
On, the thickness of film is controlled by the gap of electronic control pressing die head outlet；
(4) polyimide film by step (3) by extrusion coated film forming is sent into imidization furnace, carries out imidization processing,
Finally by cold cycling treatment repeatedly, final products are obtained；The time interval of the cold cycling treatment repeatedly is 11s, cold
Circulating temperature is 42 DEG C, and thermal cycling temperature is 166 DEG C, and cycle-index is 55 times.
Embodiment 4
A kind of cold cycling treatment Kapton repeatedly, is made: 2,2'- bis- [4- of the raw material of following parts by weight
(4- amino-benzene oxygen) phenyl] 1300 parts of hexafluoropropane, 1300 parts of 2,3,3', 4'- diphenyl ether dianhydride, 10 parts of isoquinolin, boron
50 parts of iron ore.
The preparation method of the above-mentioned Kapton of cold cycling treatment repeatedly carries out in accordance with the following steps:
(1) diamines and dianhydride are mixed, catalyst is added, be heated to 70 DEG C of initiated polymerizations, stir 30h, slurry is made
Material；
(2) paigeite is crushed, is milled, cross 130 meshes, be put into the slurry of step (1) preparation, stir evenly, be made
Coating liquid；
(3) coating liquid by step (2) preparation is sent into extrusion coating machine, and coating liquid is applied to steel band by extrusion die
On, the thickness of film is controlled by the gap of electronic control pressing die head outlet；
(4) polyimide film by step (3) by extrusion coated film forming is sent into imidization furnace, carries out imidization processing,
Finally by cold cycling treatment repeatedly, final products are obtained；The time interval of the cold cycling treatment repeatedly is 14s, cold
Circulating temperature is 44 DEG C, and thermal cycling temperature is 161 DEG C, and cycle-index is 52 times.
Comparative example 1
A kind of cold cycling treatment Kapton repeatedly, is made: 3,3 '-dimethyl of the raw material of following parts by weight
1300 parts of benzidine, 3,3 ', 4,4 ' -1300 parts of biphenyltetracarboxylic dianhydrides, 15 parts of triethylamine.
The preparation method of the above-mentioned Kapton of cold cycling treatment repeatedly carries out in accordance with the following steps:
(1) by 3,3 '-dimethylbenzidines and 3, triethylamine, heating is added in the mixing of 3 ', 4,4 '-biphenyltetracarboxylic dianhydrides
To 80 DEG C of initiated polymerizations, for 24 hours, slurry is made in stirring；
(2) slurry by step (1) preparation is sent into extrusion coating machine, and slurry is applied on steel band by extrusion die,
The thickness of film is controlled by the gap of electronic control pressing die head outlet；
(3) polyimide film by step (2) by extrusion coated film forming is sent into imidization furnace, carries out imidization processing,
Finally by cold cycling treatment repeatedly, final products are obtained；The time interval of the cold cycling treatment repeatedly is 12s, cold
Circulating temperature is 42 DEG C, and thermal cycling temperature is 165 DEG C, and cycle-index is 50 times.
Comparative example 2
A kind of Kapton is made of the raw material of following parts by weight: 3,3 ' -1300 parts of dimethylbenzidines, and 3,
3 ', 4,4 ' -1300 parts of biphenyltetracarboxylic dianhydrides, 15 parts of triethylamine, 40 parts of paigeite.
The preparation method of above-mentioned Kapton carries out in accordance with the following steps:
(1) by 3,3 '-dimethylbenzidines and 3, triethylamine, heating is added in the mixing of 3 ', 4,4 '-biphenyltetracarboxylic dianhydrides
To 80 DEG C of initiated polymerizations, for 24 hours, slurry is made in stirring；
(2) paigeite is crushed, is milled, cross 120 meshes, be put into the slurry of step (1) preparation, stir evenly, be made
Coating liquid；
(3) coating liquid by step (2) preparation is sent into extrusion coating machine, and coating liquid is applied to steel band by extrusion die
On, the thickness of film is controlled by the gap of electronic control pressing die head outlet；
(4) polyimide film by step (3) by extrusion coated film forming is sent into imidization furnace, carries out imidization processing,
Obtain final products.
Experimental example 1: bending resistance experiment
Bending resistance is the film test piece using MIT folding strength testing machine, to 15mm × 100mm specification, applies tension 10N
Afterwards, link the jig of radius 38mm, and bent repeatedly with 135 ° of angle, until fractureing, calculate bending number, test knot
Fruit is shown in Table 1:
Table 1
Note: * represents P < 0.05, * * compared with embodiment 1 and represents P < 0.01.
Experimental example 2: alkali resistance experiment
The operation of alkali resistance assessment of indices is as follows: 40mm × 40mm specification is made in the product of embodiment 1-4 and comparative example 1-2
Film test piece, weighing initial stage weight be set as W0.Film test piece is impregnated in 5% NaOH aqueous solution at 60 DEG C, in dipping
After 20 hours, test piece is taken out, is cleaned, is made it dry at 120 DEG C 30 hours with pure water, weight is measured, is set to W1, foundation
Following formula calculates:
Alkaline-resisting sex index (%)=[1- (W0-W1)/W0]X100
Test result is shown in Table 2:
Table 2
Note: * represents P < 0.05 compared with embodiment 1.
Claims (6)
1. a kind of cold cycling treatment Kapton repeatedly, which is characterized in that be made of the raw material of following parts by weight: two
1000-1500 parts of amine, 1000-1500 parts of dianhydride, 10-20 parts of catalyst, 30-50 parts of paigeite.
2. cold cycling treatment Kapton repeatedly according to claim 1, which is characterized in that the diamines is 3,
3 '-dimethylbenzidines, 4,4 '-diaminobenzophenones, 2,4- diamino -6- chlorotoluenes, 2,2'- bis- [4- (4- aminobenzene oxygen
Base) phenyl] hexafluoropropane, 2,2'- bis- [4- (4- amino-benzene oxygen) phenyl] propane or bis- (4- amino-benzene oxygen) benzene of Isosorbide-5-Nitrae-.
3. cold cycling treatment Kapton repeatedly according to claim 1, which is characterized in that the dianhydride is 3,
3 ', 4,4 '-biphenyltetracarboxylic dianhydrides, Isosorbide-5-Nitrae, 5,8- naphthalene tetracarboxylic acid dianhydrides, phenanthrene -1,8,9,10- tetracarboxylic dianhydrides, 3,4,3', 4'-
Diphenyl ether dianhydride or 2,3,3', 4'- diphenyl ether dianhydride.
4. cold cycling treatment Kapton repeatedly according to claim 1, which is characterized in that the catalyst is three
Ethamine, N, N- dimethyl cyclohexyl amine, N, N- dimethyl benzylamine, triethanolamine, N, N- dimethylethanolamine or isoquinolin.
5. a kind of preparation method of cold cycling treatment Kapton repeatedly, which is characterized in that carry out in accordance with the following steps:
(1) diamines and dianhydride are mixed, catalyst is added, be heated to 50-100 DEG C of initiated polymerization, stir 12-36h, be made
Slurry；
(2) paigeite is crushed, is milled, cross 100-160 mesh, be put into the slurry of step (1) preparation, stir evenly, be made
Coating liquid；
(3) coating liquid by step (2) preparation is sent into extrusion coating machine, and coating liquid is applied on steel band by extrusion die,
The thickness of film is controlled by the gap of electronic control pressing die head outlet；
(4) polyimide film by step (3) by extrusion coated film forming is sent into imidization furnace, carries out imidization processing, finally
By cold cycling treatment repeatedly, final products are obtained.
6. the preparation method of cold cycling treatment Kapton repeatedly according to claim 5, which is characterized in that described
The time interval of cold cycling treatment is 10-15s repeatedly, and SAPMAC method temperature is 40-45 DEG C, and thermal cycling temperature is 160-170 DEG C,
Cycle-index is 40-60 times.
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Application publication date: 20191015 |