CN109385089A - A kind of stringent equimolar monomer combines the synthesis of polyamic acid resin of compensation charging - Google Patents
A kind of stringent equimolar monomer combines the synthesis of polyamic acid resin of compensation charging Download PDFInfo
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- CN109385089A CN109385089A CN201811282967.8A CN201811282967A CN109385089A CN 109385089 A CN109385089 A CN 109385089A CN 201811282967 A CN201811282967 A CN 201811282967A CN 109385089 A CN109385089 A CN 109385089A
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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
- C08K2201/00—Specific properties of additives
- C08K2201/011—Nanostructured additives
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/02—Elements
- C08K3/04—Carbon
- C08K3/041—Carbon nanotubes
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Abstract
The invention discloses the synthesis of polyamic acid resin that a kind of stringent equimolar monomer combines compensation charging.In such a way that stringent equimolar monomer combines compensation charging, pass through extrusion coated simultaneously, biaxial oriented stretch is orientated in length and breadth, cold cycling treatment repeatedly prepares Kapton, the Kapton high mechanical strength of preparation, shrinking percentage is low, heat resistance is good, is able to satisfy the high-end requirement of electric apparatus insulation and the common requirement in lapping electromagnetic wire field and flexible circuit preparation.
Description
Technical field
The invention belongs to Kapton preparation technical fields, and in particular to a kind of stringent equimolar monomer combination compensation
The synthesis of polyamic acid resin of charging.
Background technique
Currently, the main application fields of domestic Kapton are electric apparatus insulation and lapping electromagnetic wire.Polyamides is sub-
Amine film is the key that electric apparatus insulating materials, is widely used in equipment for power transmission and distribution, wind power plant, variable-frequency motor, height
The manufacture of fast traction electric machine and high-tension transformer etc., occupies unique status in currently used electric insulation film.Last century
Since the nineties, high-performance polyimide film material becomes the key material of micro-electronic manufacturing and encapsulation again, is widely applied
In the manufacture of super large-scale integration, flexible encapsulating substrate, flexible link belt line etc..From 300 kilometers of high-speed rail of speed per hour
Kapton is all be unable to do without to electronic products such as the laptop of meagre miniaturization, mobile phone, camera, video cameras.According to
Statistics, the annual requirement of last year China's Kapton is more than 2800 tons, and the product of the offshore companies such as America and Japan accounts for city, China
The 80% of market share.And the production technology of high-performance polyimide film therein mainly rests in the developed countries such as America and Japan hand
In.The standard type Kapton of DuPont Corporation be always held in nearly 10 years time about 1000 yuans/
Kilogram high monopolization price on.
Using Kapton as substrate, in its single side or two-sided painting perfluoroethylene-propylene emulsion, adhesive tape is made can
Surround on bare copper wire, heat-resist, thickness of insulating layer is uniform and thin, good airproof performance, improves the humidity resistance of conducting wire, electrically
Energy.
But current Kapton is flexible poor, physical property and sealing performance decline, uncomfortable under the high temperature conditions
Close the preparation of high-end product such as flexible circuit board.
Summary of the invention
The purpose of the present invention is to provide the polyamic acid resin synthesis that a kind of stringent equimolar monomer combines compensation charging
Method.
A kind of stringent equimolar monomer combines the synthesis of polyamic acid resin of compensation charging, in accordance with the following steps into
Row:
(1) aromatic diamine of equimolar number, tetracarboxylic dianhydride are mixed, catalyst of triethylamine is added, is heated to 30-80
DEG C initiated polymerization stirs 2-24h, and slurry is made；
(2) carbon nanotube is added into slurry, is uniformly mixed, composite mortar is made；
(3) composite mortar made of step (2) is sent into extrusion coating machine, by extrusion die by polyimide resin liquid
It is applied on steel band, 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,
Biaxial oriented stretch in length and breadth is carried out simultaneously to be orientated, and finally by cold cycling treatment repeatedly, obtains final products.
The aromatic diamine be m-phenylene diamine (MPD), p-phenylenediamine, 3,3 '-dimethylbenzidines, 2,5- diaminotoluenes, 4,
4 '-diaminobenzophenones or 2,4- diamino -6- chlorotoluene.
The tetracarboxylic dianhydride be 3,3 ', 4,4 '-benzophenone tetracarboxylic dianhydrides, pyromellitic acid anhydride, 3,3 ', 4,4 '-
Biphenyltetracarboxylic dianhydride, 2,2 ', 3,3 '-biphenyltetracarboxylic dianhydrides, Isosorbide-5-Nitrae, 5,8- naphthalene tetracarboxylic acid dianhydrides, 1,2,5,6- naphthalene tetracarboxylic acid
Dianhydride, phenanthrene -1,8,9,10- tetracarboxylic dianhydrides or benzene -1,2,3,4- tetracarboxylic dianhydrides.
Step (3) film with a thickness of 15-25um.
The longitudinal stretching multiplying power of the orientation of biaxial oriented stretch in length and breadth is 1.8-2.8, cross directional stretch multiplying power 5.0-
9.2。
The time interval of the cold cycling treatment repeatedly is 6-12s, and SAPMAC method temperature is 30-50 DEG C, thermal cycling temperature
It is 155-185 DEG C, cycle-index is 20-50 times.
The triethylamine for accounting for total weight of the mixture 0.1-0.5% is added in step (1).
Beneficial effects of the present invention: the present invention prepares polyamides in such a way that stringent equimolar monomer combines compensation charging
Imines film, the Kapton high mechanical strength of preparation, shrinking percentage is low, and heat resistance is good, is able to satisfy electric apparatus insulation
The high-end requirement of common requirement and flexible circuit preparation with lapping electromagnetic wire field.
Specific embodiment
The present invention will be further described combined with specific embodiments below.
Embodiment 1
A kind of stringent equimolar monomer combines the synthesis of polyamic acid resin of compensation charging, in accordance with the following steps into
Row:
(1) by the m-phenylene diamine (MPD) of equimolar number, 3,0.1% catalysis is added in 3 ', 4,4 '-benzophenone tetracarboxylic dianhydrides mixing
Agent triethylamine is heated to 50 DEG C of initiated polymerizations, stirs 12h, and slurry is made；
(2) 1% carbon nanotube is added into slurry, is uniformly mixed, composite mortar is made；
(3) composite mortar made of step (2) is sent into extrusion coating machine, by extrusion die by polyimide resin liquid
It is applied on steel band, the thickness of film is controlled by the gap of electronic control pressing die head outlet；Film with a thickness of 18um；
(4) polyimide film by step (3) by extrusion coated film forming is sent into imidization furnace, carries out imidization processing,
Biaxial oriented stretch in length and breadth is carried out simultaneously to be orientated, and finally by cold cycling treatment repeatedly, obtains final products；It is described double in length and breadth
The longitudinal stretching multiplying power of axis orientation stretching orientation is 2.2, cross directional stretch multiplying power 6.2；The cold cycling treatment repeatedly when
Between between be divided into 8s, SAPMAC method temperature is 40 DEG C, and thermal cycling temperature is 175 DEG C, and cycle-index is 30 times.
Embodiment 2
A kind of stringent equimolar monomer combines the synthesis of polyamic acid resin of compensation charging, in accordance with the following steps into
Row:
(1) the 3 of equimolar number, 3 '-dimethylbenzidines, pyromellitic acid anhydride are mixed, 0.2% catalyst three is added
Ethamine is heated to 30 DEG C of initiated polymerizations, stirs 8h, and slurry is made；
(2) 1% carbon nanotube is added into slurry, is uniformly mixed, composite mortar is made；
(3) composite mortar made of step (2) is sent into extrusion coating machine, by extrusion die by polyimide resin liquid
It is applied on steel band, the thickness of film is controlled by the gap of electronic control pressing die head outlet；Film with a thickness of 15um；
(4) polyimide film by step (3) by extrusion coated film forming is sent into imidization furnace, carries out imidization processing,
Biaxial oriented stretch in length and breadth is carried out simultaneously to be orientated, and finally by cold cycling treatment repeatedly, obtains final products；It is described double in length and breadth
The longitudinal stretching multiplying power of axis orientation stretching orientation is 1.8, cross directional stretch multiplying power 5.0；The cold cycling treatment repeatedly when
Between between be divided into 6s, SAPMAC method temperature is 30 DEG C, and thermal cycling temperature is 155 DEG C, and cycle-index is 20 times.
Embodiment 3
A kind of stringent equimolar monomer combines the synthesis of polyamic acid resin of compensation charging, in accordance with the following steps into
Row:
(1) by 2,5- diaminotoluene, the phenanthrene -1,8 of equimolar number, 9,10- tetracarboxylic dianhydrides mixing is added 0.5% and urges
Agent triethylamine, is heated to 80 DEG C of initiated polymerizations, and for 24 hours, slurry is made in stirring；
(2) 1% carbon nanotube is added into slurry, is uniformly mixed, composite mortar is made；
(3) composite mortar made of step (2) is sent into extrusion coating machine, by extrusion die by polyimide resin liquid
It is applied on steel band, the thickness of film is controlled by the gap of electronic control pressing die head outlet；Film with a thickness of 25um；
(4) polyimide film by step (3) by extrusion coated film forming is sent into imidization furnace, carries out imidization processing,
Biaxial oriented stretch in length and breadth is carried out simultaneously to be orientated, and finally by cold cycling treatment repeatedly, obtains final products；It is described double in length and breadth
The longitudinal stretching multiplying power of axis orientation stretching orientation is 2.8, cross directional stretch multiplying power 9.2；The cold cycling treatment repeatedly when
Between between be divided into 12s, SAPMAC method temperature is 50 DEG C, and thermal cycling temperature is 185 DEG C, and cycle-index is 50 times.
Embodiment 4
A kind of stringent equimolar monomer combines the synthesis of polyamic acid resin of compensation charging, in accordance with the following steps into
Row:
(1) by the m-phenylene diamine (MPD) of equimolar number, 3,0.1% catalysis is added in 3 ', 4,4 '-benzophenone tetracarboxylic dianhydrides mixing
Agent triethylamine is heated to 50 DEG C of initiated polymerizations, stirs 12h, and slurry is made；
(2) 1% carbon nanotube is added into slurry, 1%4- [trans- 4- (trans- 4- propylcyclohexyl) cyclohexyl] toluene mixes
It closes uniformly, composite mortar is made；
(3) composite mortar made of step (2) is sent into extrusion coating machine, by extrusion die by polyimide resin liquid
It is applied on steel band, the thickness of film is controlled by the gap of electronic control pressing die head outlet；Film with a thickness of 18um；
(4) polyimide film by step (3) by extrusion coated film forming is sent into imidization furnace, carries out imidization processing,
Biaxial oriented stretch in length and breadth is carried out simultaneously to be orientated, and finally by cold cycling treatment repeatedly, obtains final products；It is described double in length and breadth
The longitudinal stretching multiplying power of axis orientation stretching orientation is 2.2, cross directional stretch multiplying power 6.2；The cold cycling treatment repeatedly when
Between between be divided into 8s, SAPMAC method temperature is 40 DEG C, and thermal cycling temperature is 175 DEG C, and cycle-index is 30 times.
Embodiment 5
A kind of stringent equimolar monomer combines the synthesis of polyamic acid resin of compensation charging, in accordance with the following steps into
Row:
(1) by the m-phenylene diamine (MPD) of equimolar number, 3,0.1% catalysis is added in 3 ', 4,4 '-benzophenone tetracarboxylic dianhydrides mixing
Agent triethylamine is heated to 50 DEG C of initiated polymerizations, stirs 12h, and slurry is made；
(2) 1% carbon nanotube, 1%Sr Be Eu are added into slurry2O5Crystal powder is uniformly mixed, composite pulp is made
Material；
(3) composite mortar made of step (2) is sent into extrusion coating machine, by extrusion die by polyimide resin liquid
It is applied on steel band, the thickness of film is controlled by the gap of electronic control pressing die head outlet；Film with a thickness of 18um；
(4) polyimide film by step (3) by extrusion coated film forming is sent into imidization furnace, carries out imidization processing,
Biaxial oriented stretch in length and breadth is carried out simultaneously to be orientated, and finally by cold cycling treatment repeatedly, obtains final products；It is described double in length and breadth
The longitudinal stretching multiplying power of axis orientation stretching orientation is 2.2, cross directional stretch multiplying power 6.2；The cold cycling treatment repeatedly when
Between between be divided into 8s, SAPMAC method temperature is 40 DEG C, and thermal cycling temperature is 175 DEG C, and cycle-index is 30 times.
Embodiment 6
A kind of stringent equimolar monomer combines the synthesis of polyamic acid resin of compensation charging, in accordance with the following steps into
Row:
(1) by the m-phenylene diamine (MPD) of equimolar number, 3,0.1% catalysis is added in 3 ', 4,4 '-benzophenone tetracarboxylic dianhydrides mixing
Agent triethylamine is heated to 50 DEG C of initiated polymerizations, stirs 12h, and slurry is made；
(2) 1% carbon nanotube, 1%K (Al Ge are added into slurry3O8) crystal powder, it is uniformly mixed, composite pulp is made
Material；
(3) composite mortar made of step (2) is sent into extrusion coating machine, by extrusion die by polyimide resin liquid
It is applied on steel band, the thickness of film is controlled by the gap of electronic control pressing die head outlet；Film with a thickness of 18um；
(4) polyimide film by step (3) by extrusion coated film forming is sent into imidization furnace, carries out imidization processing,
Biaxial oriented stretch in length and breadth is carried out simultaneously to be orientated, and finally by cold cycling treatment repeatedly, obtains final products；It is described double in length and breadth
The longitudinal stretching multiplying power of axis orientation stretching orientation is 2.2, cross directional stretch multiplying power 6.2；The cold cycling treatment repeatedly when
Between between be divided into 8s, SAPMAC method temperature is 40 DEG C, and thermal cycling temperature is 175 DEG C, and cycle-index is 30 times.
Experimental example:
Referring to the requirement of international standard IEC 60674-3-4/6:1993: 150 DEG C, 400 DEG C of shrinking percentage≤0.06%, volume
Resistivity >=1012Ω .m, surface resistivity >=1014Ω.150 DEG C for detecting 1-6 of the embodiment of the present invention, 400 DEG C of shrinking percentages, body
Product resistivity and surface resistivity, testing result are as shown in Table 1 and Table 2.
Table 1
Note: * represents P < 0.05 compared with example 1 group.
150 DEG C of embodiment 1-6 as can be seen from Table 1,400 DEG C of shrinking percentages are respectively less than 0.06%, meet international standard IEC
The requirement of 60674-3-4/6:1993；150 DEG C of embodiment 4-5,400 DEG C of shrinking percentages are significantly better than embodiment 1, and effect is more
It is excellent.
Table 2
Note: * represents P < 0.05 compared with example 1 group.
As can be seen from Table 2, embodiment 1-6 volume resistivity is greater than 1012Ω .m, surface resistivity are greater than 1014Ω is full
The requirement of sufficient international standard IEC 60674-3-4/6:1993；The volume resistivity of embodiment 4-5, surface resistivity are significant excellent
In embodiment 1, effect is more excellent.
Claims (7)
1. the synthesis of polyamic acid resin that a kind of stringent equimolar monomer combines compensation charging, which is characterized in that according to such as
Lower step carries out:
(1) aromatic diamine of equimolar number, tetracarboxylic dianhydride are mixed, catalyst of triethylamine is added, is heated to 30-80 DEG C and draws
Polymerization reaction is sent out, 2-24h is stirred, slurry is made；
(2) carbon nanotube is added into slurry, is uniformly mixed, composite mortar is made；
(3) composite mortar made of step (2) is sent into extrusion coating machine, is coated with polyimide resin liquid by extrusion die
Onto steel band, 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, simultaneously
It carries out biaxial oriented stretch in length and breadth to be orientated, finally by cold cycling treatment repeatedly, obtains final products.
2. stringent equimolar monomer combines the synthesis of polyamic acid resin of compensation charging according to claim 1, special
Sign is, the aromatic diamine is m-phenylene diamine (MPD), p-phenylenediamine, 3,3 '-dimethylbenzidines, 2,5- diaminotoluenes, 4,
4 '-diaminobenzophenones or 2,4- diamino -6- chlorotoluene.
3. stringent equimolar monomer combines the synthesis of polyamic acid resin of compensation charging according to claim 1, special
Sign is that the tetracarboxylic dianhydride is 3,3 ', 4,4 '-benzophenone tetracarboxylic dianhydrides, pyromellitic acid anhydride, 3,3 ', 4,4 '-connection
Benzene tertacarbonic acid's dianhydride, 2,2 ', 3,3 '-biphenyltetracarboxylic dianhydrides, Isosorbide-5-Nitrae, 5,8- naphthalene tetracarboxylic acid dianhydrides, 1,2,5,6- naphthalene tetracarboxylic acid two
Acid anhydride, phenanthrene -1,8,9,10- tetracarboxylic dianhydrides or benzene -1,2,3,4- tetracarboxylic dianhydrides.
4. stringent equimolar monomer combines the synthesis of polyamic acid resin of compensation charging according to claim 1, special
Sign is, step (3) film with a thickness of 15-25um.
5. stringent equimolar monomer combines the synthesis of polyamic acid resin of compensation charging according to claim 1, special
Sign is that the longitudinal stretching multiplying power of the orientation of biaxial oriented stretch in length and breadth is 1.8-2.8, cross directional stretch multiplying power 5.0-9.2.
6. stringent equimolar monomer combines the synthesis of polyamic acid resin of compensation charging according to claim 1, special
Sign is that the time interval of the cold cycling treatment repeatedly is 6-12s, and SAPMAC method temperature is 30-50 DEG C, and thermal cycling temperature is
155-185 DEG C, cycle-index is 20-50 times.
7. stringent equimolar monomer combines the synthesis of polyamic acid resin of compensation charging according to claim 1, special
Sign is, the triethylamine for accounting for total weight of the mixture 0.1-0.5% is added in step (1).
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110330791A (en) * | 2019-08-06 | 2019-10-15 | 江苏亚宝绝缘材料股份有限公司 | A kind of preparation method and product of the Kapton of cold cycling treatment repeatedly |
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| US20100279095A1 (en) * | 2007-10-17 | 2010-11-04 | Agency For Scinece Tecnology And Research | Composite films comprising carbon nanotubes and polymer |
| US20110003965A1 (en) * | 2009-07-01 | 2011-01-06 | National Taiwan University | Cnt-pi complex having emi shielding effectiveness and method for producing the same |
| CN104448312A (en) * | 2014-11-27 | 2015-03-25 | 北京化工大学常州先进材料研究院 | High-dielectric-constant polyimide film provided with multiwalled carbon nanotubes and preparation method of high-dielectric-constant polyimide film |
| CN106893121A (en) * | 2015-12-17 | 2017-06-27 | 深圳瑞华泰薄膜科技有限公司 | A kind of Dimensionally-stablepolyimide polyimide film high and preparation method thereof |
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| US20100279095A1 (en) * | 2007-10-17 | 2010-11-04 | Agency For Scinece Tecnology And Research | Composite films comprising carbon nanotubes and polymer |
| US20110003965A1 (en) * | 2009-07-01 | 2011-01-06 | National Taiwan University | Cnt-pi complex having emi shielding effectiveness and method for producing the same |
| CN104448312A (en) * | 2014-11-27 | 2015-03-25 | 北京化工大学常州先进材料研究院 | High-dielectric-constant polyimide film provided with multiwalled carbon nanotubes and preparation method of high-dielectric-constant polyimide film |
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| CN110330791A (en) * | 2019-08-06 | 2019-10-15 | 江苏亚宝绝缘材料股份有限公司 | A kind of preparation method and product of the Kapton of cold cycling treatment repeatedly |
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Application publication date: 20190226 Assignee: YANGZHOU YABAO NEW MATERIAL TECHNOLOGY CO.,LTD. Assignor: JIANGSU YABAO INSULATION MATERIAL Co.,Ltd. Contract record no.: X2023980036321 Denomination of invention: A synthesis method of polyamide acid resin with strict equimolar monomer combination compensation feeding Granted publication date: 20210205 License type: Common License Record date: 20230608 |