CN110330792A - A kind of preparation method and product of the adjustable extrusion coated Kapton in part - Google Patents
A kind of preparation method and product of the adjustable extrusion coated Kapton in part Download PDFInfo
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- CN110330792A CN110330792A CN201910719639.8A CN201910719639A CN110330792A CN 110330792 A CN110330792 A CN 110330792A CN 201910719639 A CN201910719639 A CN 201910719639A CN 110330792 A CN110330792 A CN 110330792A
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- extrusion coated
- dianhydride
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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
- C08K3/02—Elements
- C08K3/04—Carbon
- C08K3/042—Graphene or derivatives, e.g. graphene oxides
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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
- C08K5/00—Use of organic ingredients
- C08K5/04—Oxygen-containing compounds
- C08K5/09—Carboxylic acids; Metal salts thereof; Anhydrides thereof
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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
- C08K5/00—Use of organic ingredients
- C08K5/16—Nitrogen-containing compounds
- C08K5/17—Amines; Quaternary ammonium compounds
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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
- C08K9/00—Use of pretreated ingredients
- C08K9/04—Ingredients treated with organic substances
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- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Processing And Handling Of Plastics And Other Materials For Molding In General (AREA)
- Macromolecular Compounds Obtained By Forming Nitrogen-Containing Linkages In General (AREA)
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Abstract
The invention discloses the preparation method and product of a kind of adjustable extrusion coated Kapton in part, the substance including following parts by weight: 400-600 parts of polyimides, 50-80 parts of trifluoroacetic anhydride, 10-15 parts of triethylamine, 6-15 parts of graphene.Kapton prepared by the present invention, it is prepared using the method for adjustable extrusion coated, the Kapton with graded thickness can be prepared, the addition of component trifluoroacetic anhydride and triethylamine, both it so that dispersion of the graphene in preparation stoste is more uniform, and can further can be reacted with polyimides with modified graphene, the molecular gap for infiltrating through polyimides enhances the resistance to shrinkage of film.
Description
Technical field
The invention belongs to Kapton technical fields, and in particular to a kind of adjustable extrusion coated polyimides in part
The preparation method and product of film.
Background technique
Kapton is earliest one of the commodity of polyimides, and the slot insulation and cable for motor are around packaging material.
Kapton is because its mechanical dimensional stability and thermal dimensional stability are excellent, and the characteristic with chemical stability, therefore by
It is widely used in Material for electrical/electroniuse use, universe/aviation and is electrically communicated field.
Polyimides chemical property is stablized, and polyimides does not need addition fire retardant and prevents from burning, general poly-
The all anti-chemical solvent of acid imide such as hydro carbons, esters, ethers, alcohols and dichlorodifluoromethan.Polyimides is that comprehensive performance is optimal organic
One of high molecular material, high temperature resistant is up to 400 DEG C or more, -200~300 DEG C of long-term use temperature range, partially without sharp melting point
Graphene be one kind by carbon atom with sp2Hybridized orbit forms the Two-dimensional Carbon nanometer material that hexangle type is in honeycomb lattice
Material.Graphene has excellent optics, electricity, mechanical characteristic, passes in materialogy, micro-nano technology, the energy, biomedicine and drug
Pass etc. is with important application prospects.Graphene is added directly into progress extrusion coated film forming in polyimides film liquid, point
It dissipates unevenly, influences the heating conduction and thermal contraction performance of final products.
Summary of the invention
The purpose of the present invention is to provide the preparation methods and system of a kind of adjustable extrusion coated Kapton in part
Product.
A kind of adjustable extrusion coated Kapton in part, the substance including following parts by weight: polyimides
400-600 parts, 50-80 parts of trifluoroacetic anhydride, 10-15 parts of triethylamine, 6-15 parts of graphene.
Trifluoroacetic anhydride and triethylamine, can be with dispersed graphite alkene, so that it is distributed in system in preparing material system
More uniform, trifluoroacetic anhydride is also used as dehydrating agent, and triethylamine and reacts incomplete polyamides as catalyst in system
Secondary response, the anti-contracility energy of enhanced film material occur for imines.
The polyimides the preparation method comprises the following steps: using diamines and dianhydride as raw material, be made using two step solution polycondensations.
The diamines is hydroquinone di ether diamines, in diphenyldiamine, diphenylmethane diamine, two ether diamine of bisphenol-A
It is one or more kinds of.
The dianhydride is benzophenone dianhydride, two ether dianhydride of triphen, hydroquinone di ether dianhydride, diphenyl ether dianhydride, isophthalic two
One of two ether dianhydride of phenol or more than one.
The preparation method of the above-mentioned adjustable extrusion coated Kapton in part carries out in accordance with the following steps:
(1) at room temperature, diamines and dianhydride are added to reaction kettle, metacresol is added under nitrogen protection, after mixing evenly,
Isoquinolin is added, is warming up to 180-200 DEG C, reacts 10-14 hours, reaction solution is poured into ethyl alcohol after cooling and is precipitated, polyamides is made
Imide resin；
(2) trifluoroacetic anhydride and triethylamine are mixed, is put into graphene, it is pre- after high shear dispersion machine is subject to high-temperature process
First disperse, treatment temperature is 300-500 DEG C, and graphene mixed liquor is made；
(3) polyimide resin of synthesis and the agitated reaction kettle of graphene mixed liquor are stirred, mixing speed 1200-
Polyimide resin film liquid is made in 1600rpm, mixing time 2-5h；
(4) polyimide resin film liquid is sent into extrusion coating machine, is applied polyimide resin film liquid by extrusion die
On cloth to steel band, the thickness of film is controlled by the gap of electronic control pressing die head outlet；
(5) polyimide film by extrusion coated film forming is sent into imidization furnace, carries out imidization processing, finally by anti-
Multiple cold cycling treatment, obtains final products.
The gap of pressing die head outlet again during press mold can local directed complete set, have the thin of gradually thickness gradient to produce
Film.
The time interval of the cold cycling treatment repeatedly is 6-15s, and SAPMAC method temperature is 25-30 DEG C, thermal cycling temperature
It is 130-150 DEG C, cycle-index is 30-60 times.
Beneficial effects of the present invention: Kapton prepared by the present invention, using the method system of adjustable extrusion coated
It is standby to form, the Kapton with graded thickness can be prepared, the addition of component trifluoroacetic anhydride and triethylamine both can be with
Modified graphene so that dispersion of the graphene in preparation stoste is more uniform, and can further occur with polyimides anti-
It answers, infiltrates through the molecular gap of polyimides, enhance the resistance to shrinkage of film.
Specific embodiment
The present invention will be further described combined with specific embodiments below.
Embodiment 1
A kind of preparation method of the adjustable extrusion coated Kapton in part carries out in accordance with the following steps:
(1) at room temperature, 1200g diphenyldiamine and 1200g benzophenone dianhydride are added to reaction kettle, under nitrogen protection
500g isoquinolin is added after mixing evenly in 15000g metacresol between addition, is warming up to 200 DEG C, reacts 13 hours, will after cooling
Reaction solution pours into ethyl alcohol precipitation, and polyimide resin is made；
(2) trifluoroacetic anhydride 12g and triethylamine 2.5g is mixed, is put into graphene 2g, is subject to height through high shear dispersion machine
Disperse in advance after temperature processing, treatment temperature is 400 DEG C, and graphene mixed liquor is made；
(3) polyimide resin of synthesis and the agitated reaction kettle of graphene mixed liquor are stirred, mixing speed
Polyimide resin film liquid is made in 1400rpm, mixing time 3h；
(4) polyimide resin film liquid is sent into extrusion coating machine, is applied polyimide resin film liquid by extrusion die
On cloth to steel band, the thickness of film is controlled by the gap of electronic control pressing die head outlet；
(5) polyimide film by extrusion coated film forming is sent into imidization furnace, carries out imidization processing, finally by anti-
Multiple cold cycling treatment, obtains final products.
Through experimental tests, manufactured product thermal coefficient is 1.12W/ (MK), under the conditions of 85 DEG C, stores 30 days, receives
Shrinkage is 0.12%.
Embodiment 2
A kind of preparation method of the adjustable extrusion coated Kapton in part carries out in accordance with the following steps:
(1) at room temperature, two ether diamine of 1050g bisphenol-A and two ether dianhydride of 1050g resorcinol are added to reaction kettle,
460g isoquinolin is added after mixing evenly in 14000g metacresol between being added under nitrogen protection, is warming up to 190 DEG C, reaction 12 is small
When, reaction solution is poured into ethyl alcohol after cooling and is precipitated, polyimide resin is made；
(2) trifluoroacetic anhydride 11g and triethylamine 2.2g is mixed, is put into graphene 1.6g, is subject to through high shear dispersion machine
Disperse in advance after high-temperature process, treatment temperature is 450 DEG C, and graphene mixed liquor is made；
(3) polyimide resin of synthesis and the agitated reaction kettle of graphene mixed liquor are stirred, mixing speed
Polyimide resin film liquid is made in 1500rpm, mixing time 4h；
(4) polyimide resin film liquid is sent into extrusion coating machine, is applied polyimide resin film liquid by extrusion die
On cloth to steel band, the thickness of film is controlled by the gap of electronic control pressing die head outlet；
(5) polyimide film by extrusion coated film forming is sent into imidization furnace, carries out imidization processing, finally by anti-
Multiple cold cycling treatment, obtains final products.
Through experimental tests, manufactured product thermal coefficient is 1.14W/ (MK), under the conditions of 85 DEG C, stores 30 days, receives
Shrinkage is 0.11%.
Embodiment 3
A kind of preparation method of the adjustable extrusion coated Kapton in part carries out in accordance with the following steps:
(1) at room temperature, 1300g diphenylmethane diamine and 1300g hydroquinone di ether dianhydride are added to reaction kettle, nitrogen
600g isoquinolin is added after mixing evenly in 16000g metacresol between being added under gas shielded, is warming up to 180 DEG C, reacts 13 hours,
Reaction solution is poured into ethyl alcohol after cooling to be precipitated, polyimide resin is made；
(2) trifluoroacetic anhydride 13g and triethylamine 3g is mixed, is put into graphene 3g, is subject to high temperature through high shear dispersion machine
Disperse in advance after processing, treatment temperature is 600 DEG C, and graphene mixed liquor is made；
(3) polyimide resin of synthesis and the agitated reaction kettle of graphene mixed liquor are stirred, mixing speed
Polyimide resin film liquid is made in 1300rpm, mixing time 5h；
(4) polyimide resin film liquid is sent into extrusion coating machine, is applied polyimide resin film liquid by extrusion die
On cloth to steel band, the thickness of film is controlled by the gap of electronic control pressing die head outlet；
(5) polyimide film by extrusion coated film forming is sent into imidization furnace, carries out imidization processing, finally by anti-
Multiple cold cycling treatment, obtains final products.
Through experimental tests, manufactured product thermal coefficient is 1.09W/ (MK), under the conditions of 85 DEG C, stores 30 days, receives
Shrinkage is 0.13%.
Embodiment 4
A kind of preparation method of the adjustable extrusion coated Kapton in part carries out in accordance with the following steps:
(1) at room temperature, 1250g hydroquinone di ether diamines and 1250g benzophenone dianhydride are added to reaction kettle, nitrogen
430g isoquinolin is added after mixing evenly in 14000g metacresol between the lower addition of protection, is warming up to 200 DEG C, reacts 14 hours, cold
But reaction solution is poured into ethyl alcohol afterwards to be precipitated, polyimide resin is made；
(2) trifluoroacetic anhydride 12.5g and triethylamine 2.8g is mixed, is put into graphene 2.2g, adds through high shear dispersion machine
To disperse in advance after high-temperature process, treatment temperature is 400 DEG C, and graphene mixed liquor is made；
(3) polyimide resin of synthesis and the agitated reaction kettle of graphene mixed liquor are stirred, mixing speed
Polyimide resin film liquid is made in 1400rpm, mixing time 2h；
(4) polyimide resin film liquid is sent into extrusion coating machine, is applied polyimide resin film liquid by extrusion die
On cloth to steel band, the thickness of film is controlled by the gap of electronic control pressing die head outlet；
(5) polyimide film by extrusion coated film forming is sent into imidization furnace, carries out imidization processing, finally by anti-
Multiple cold cycling treatment, obtains final products.
Through experimental tests, manufactured product thermal coefficient is 1.11W/ (MK), under the conditions of 85 DEG C, stores 30 days, receives
Shrinkage is 0.11%.
Embodiment 5
A kind of preparation method of the adjustable extrusion coated Kapton in part carries out in accordance with the following steps:
(1) at room temperature, 1200g diphenyldiamine and 1200g benzophenone dianhydride are added to reaction kettle, under nitrogen protection
500g isoquinolin is added after mixing evenly in 15000g metacresol between addition, is warming up to 200 DEG C, reacts 13 hours, will after cooling
Reaction solution pours into ethyl alcohol precipitation, and polyimide resin is made；
(2) polyimide resin of synthesis and the agitated reaction kettle of graphene 2g are stirred, mixing speed 1400rpm is stirred
Time 3h is mixed, polyimide resin film liquid is made；
(3) polyimide resin film liquid is sent into extrusion coating machine, is applied polyimide resin film liquid by extrusion die
On cloth to steel band, the thickness of film is controlled by the gap of electronic control pressing die head outlet；
(4) polyimide film by extrusion coated film forming is sent into imidization furnace, carries out imidization processing, finally by anti-
Multiple cold cycling treatment, obtains final products.
Through experimental tests, manufactured product thermal coefficient is 1.54W/ (MK), under the conditions of 85 DEG C, stores 30 days, receives
Shrinkage is 0.21%.
Embodiment 6
A kind of preparation method of the adjustable extrusion coated Kapton in part carries out in accordance with the following steps:
(1) at room temperature, 1200g diphenyldiamine and 1200g benzophenone dianhydride are added to reaction kettle, under nitrogen protection
500g isoquinolin is added after mixing evenly in 15000g metacresol between addition, is warming up to 200 DEG C, reacts 13 hours, will after cooling
Reaction solution pours into ethyl alcohol precipitation, and polyimide resin is made；
(2) trifluoroacetic anhydride 12g and triethylamine 2.5g is mixed, is divided in advance after high shear dispersion machine is subject to high-temperature process
It dissipates, treatment temperature is 400 DEG C, and mixed liquor is made；
(3) polyimide resin of synthesis and the agitated reaction kettle of mixed liquor are stirred, mixing speed 1400rpm, stirring
Polyimide resin film liquid is made in time 3h；
(4) polyimide resin film liquid is sent into extrusion coating machine, is applied polyimide resin film liquid by extrusion die
On cloth to steel band, the thickness of film is controlled by the gap of electronic control pressing die head outlet；
(5) polyimide film by extrusion coated film forming is sent into imidization furnace, carries out imidization processing, finally by anti-
Multiple cold cycling treatment, obtains final products.
Through experimental tests, manufactured product thermal coefficient is 1.63W/ (MK), under the conditions of 85 DEG C, stores 30 days, receives
Shrinkage is 0.28%.
Claims (7)
1. a kind of adjustable extrusion coated Kapton in part, which is characterized in that the substance including following parts by weight: poly-
400-600 parts of acid imide, 50-80 parts of trifluoroacetic anhydride, 10-15 parts of triethylamine, 6-15 parts of graphene.
2. the adjustable extrusion coated Kapton in part according to claim 1, which is characterized in that the polyimides
The preparation method comprises the following steps: using diamines and dianhydride as raw material, be made using two step solution polycondensations.
3. the adjustable extrusion coated Kapton in part according to claim 1, which is characterized in that the diamines be for
One of hydroquinone di ether diamines, diphenyldiamine, diphenylmethane diamine, two ether diamine of bisphenol-A or more than one.
4. the adjustable extrusion coated Kapton in part according to claim 1, which is characterized in that the dianhydride is two
One of benzophenone dianhydride, two ether dianhydride of triphen, hydroquinone di ether dianhydride, diphenyl ether dianhydride, two ether dianhydride of resorcinol or
More than one.
5. the preparation method of the adjustable extrusion coated Kapton in part described in claim 1, which is characterized in that according to such as
Lower step carries out:
(1) at room temperature, diamines and dianhydride are added to reaction kettle, metacresol is added under nitrogen protection, after mixing evenly, be added
Isoquinolin is warming up to 180-200 DEG C, reacts 10-14 hours, and reaction solution is poured into ethyl alcohol after cooling and is precipitated, polyimides is made
Resin；
(2) trifluoroacetic anhydride and triethylamine are mixed, is put into graphene, divides in advance after high shear dispersion machine is subject to high-temperature process
It dissipates, treatment temperature is 300-500 DEG C, and graphene mixed liquor is made；
(3) polyimide resin of synthesis and the agitated reaction kettle of graphene mixed liquor are stirred, mixing speed 1200-
Polyimide resin film liquid is made in 1600rpm, mixing time 2-5h；
(4) polyimide resin film liquid is sent into extrusion coating machine, is applied to polyimide resin film liquid by extrusion die
On steel band, the thickness of film is controlled by the gap of electronic control pressing die head outlet；
(5) polyimide film by extrusion coated film forming is sent into imidization furnace, carries out imidization processing, finally by repeatedly cold
Thermal cycle processing, obtains final products.
6. the preparation method of the adjustable extrusion coated Kapton in part according to claim 5, which is characterized in that institute
State the gap of pressing die head outlet again during press mold can local directed complete set, to produce the film for having gradually thickness gradient.
7. the preparation method of the adjustable extrusion coated Kapton in part according to claim 5, which is characterized in that institute
The time interval for stating repeatedly cold cycling treatment is 6-15s, and SAPMAC method temperature is 25-30 DEG C, thermal cycling temperature 130-150
DEG C, cycle-index is 30-60 times.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112218496A (en) * | 2020-10-10 | 2021-01-12 | 江南大学 | Thermal rectifying device and application thereof in regulating graphene thermal rectifying effect |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112218496A (en) * | 2020-10-10 | 2021-01-12 | 江南大学 | Thermal rectifying device and application thereof in regulating graphene thermal rectifying effect |
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