CN114292423B - Polyimide composite film easy to cut and preparation method thereof - Google Patents
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Abstract
The invention discloses an easy-to-cut polyimide composite film and a preparation method thereof, belonging to the technical field of polyimide films. The preparation method comprises (1) preparing low molecular weight polyamic acid glue solution; (2) The inorganic filler, the coupling agent and the oligomer form strong interaction under the action of ball milling or sanding; (3) The modified inorganic filler slurry is further mixed with diamine and dianhydride to prepare high-viscosity polyamide acid composite glue solution; (4) And (3) casting the high-viscosity polyamide acid composite glue solution into a film, heating and curing to obtain the polyimide composite film. In the polyimide composite film, the polyimide resin accounts for 60-90 wt%, and the inorganic filler accounts for 10-40 wt%. Compared with the traditional polyimide film, the polyimide composite film has the advantages of low viscosity to a cutter during cutting, small cutting resistance, regular cut, lower cost and easy large-scale manufacturing.
Description
Technical Field
The invention belongs to the technical field of polyimide films, and particularly relates to an easy-to-cut polyimide composite film and a preparation method thereof.
Background
The polyimide film is a high-temperature-resistant special engineering plastic and is widely applied in the fields of aerospace, microelectronics, new energy batteries, high-speed rail wind power, smart phones and the like. Common width specifications for polyimide films are 500mm, 520mm, 1040mm, etc. In practical applications, the polyimide film needs to be cut into various shapes and sizes. Compared with materials such as ceramics, glass, metal and the like, the polymer has the problems of soft material, viscoelasticity, knife adhesion, difficulty in cutting and leveling of micro size and the like during cutting due to the fact that the high polymer bonding force is Van der Waals force and the high polymer chains are wound.
The addition of inorganic filler can improve the properties of the material such as modulus, and the like, and in the existing data, the addition of coupling agent, organic amine and other modified inorganic fillers is often combined with the polymer. Patent application CN 101260235A discloses the preparation of polyimide films by modification of inorganic clays with amino-containing silicone coupling agents, followed by polycondensation of aromatic dianhydrides, diamines in a filler solution. In the modification process, inorganic filler is required to be dispersed in a solvent, and the inorganic filler is filtered and dried after modification. Patent CN 1300251C discloses the preparation of polyimide by ultrasonic dispersion of organized clay, dissolving diamine, and then adding dianhydride for polymerization. The preparation process of the organic clay needs to use concentrated hydrochloric acid, organic amine containing siloxane chain segments and the like, and relates to the steps of filtering, washing, drying and the like.
The steps of the inorganic filler modification process are complicated, a large amount of solvent is used, the mass preparation of the polyimide film is not facilitated, and the cutting related problem is not reported.
Disclosure of Invention
Aiming at the problems in the prior art, the technical problem to be solved by the invention is to provide a polyimide composite film which is easy to cut. Another technical problem to be solved by the invention is to provide a preparation method of a polyimide composite film easy to cut. The composite film consists of polyimide resin and low-hardness inorganic filler, the preparation method is simple, mass production is facilitated, products can be cut under small force, and the cuts are parallel and level.
In order to solve the problems, the technical scheme adopted by the invention is as follows:
a preparation method of a polyimide composite film easy to cut comprises the following steps:
(1) Preparing an oligomer; adding a diamine monomer into a solvent, stirring, emulsifying and dispersing, then adding a dianhydride monomer, and stirring for 6-12 hours to obtain an oligomer glue solution; the addition amount of the dianhydride monomer is 70-90% of the molar weight of the diamine monomer, and the solid content of the oligomer glue solution is 20-40 wt%;
(2) Coating inorganic filler; adding inorganic filler and coupling agent into the oligomer glue solution obtained in the step (1), and performing sand grinding or ball milling for 6-12 hours to obtain uniform slurry; the addition amount of the oligomer glue solution is 5-20 wt% of the inorganic filler, and the addition amount of the coupling agent is 1-10 wt% of the inorganic filler; the Mohs hardness of the inorganic filler is lower than 3, and the particle size is 500 nm-15 mu m;
(3) Preparing a composite glue solution; adding a diamine monomer into a solvent, stirring and dissolving, adding the slurry obtained in the step (2) for emulsification, and then adding a dianhydride monomer for polycondensation reaction to obtain a composite glue solution; the solid content of the composite glue solution is 5-30 wt%, and the apparent viscosity is 5000-300000 mPas.S;
(4) Preparing a polyimide composite film: and (4) carrying out tape casting film formation on the composite glue solution obtained in the step (3), and then heating and curing to obtain a finished polyimide composite film.
The preparation method of the easy-to-cut polyimide composite film comprises the step (2), wherein the addition amount of the oligomer glue solution is 8-15 wt% of the mass of the inorganic filler, and the addition amount of the coupling agent is 2-6 wt% of the mass of the inorganic filler; the coupling agent is one or a mixture of more of gamma-aminopropyltriethoxysilane KH550, gamma-glycidoxypropyltrimethoxysilane KH560 or gamma-methacryloxypropyltrimethoxysilane KH 570.
The preparation method of the easy-to-cut polyimide composite film comprises the step (2), wherein the addition amount of the oligomer glue solution is 10-12 wt% of the mass of the inorganic filler, and the addition amount of the coupling agent is 3-5 wt% of the mass of the inorganic filler.
The preparation method of the easy-to-cut polyimide film comprises the step (3) of controlling the adding amount of the slurry to 10-40 wt% of the inorganic filler and 60-90 wt% of the polymer resin in the finished polyimide composite film; the solid content of the composite glue solution is 15-20 wt%, and the apparent viscosity is 30000-60000 mPas.
The preparation method of the polyimide film easy to cut comprises the step (3), wherein the addition amount of the slurry is controlled to be 15-30 wt% of the inorganic filler and 70-85 wt% of the polymer resin in the finished polyimide composite film.
The preparation method of the easy-to-cut polyimide composite film comprises the step (4), wherein the temperature for heating and curing is 200-400 ℃, the length of a drying tunnel is 20-30 m, the speed of casting equipment is 2.5-10 m/min, the time of the whole film drying process is 6-24 min, and the thickness of the finished polyimide composite film is 5-150 mu m.
<xnotran> , , ,4,4' - ,4,4' - ,1,3- (4 ' - ) ,1,4- (4- ) ,2,2 ' - ( ) ,4,4' - -2,2' - -1,1' - (M-Tolidine), 4,4' - ,2,2 ' - [4- (4- ) ] ,2- (4- ) -5- , ,3,3' - ,4,4' - ,2 2' - ,4,4- ,4,4' - (3- ) ,4,4' - (4- ) 4,4' - (3- ) 2,2- [4- (4- ) ] ; </xnotran>
<xnotran> (PMDA), 3,3',4,4' - ,2,3,3 ',4' - ,3,3',4,4' - ,4,4'- ,2,3,3', 4'- ,2,2 ` - (3,4- ) ,1,2,4,5- , -3,4,3',4'- ,4,4' - ,9,9- (3,4- ) ,3,3,4,4- ,4,4'- (4,4' - ) (BPADA) - - ; </xnotran>
The solvent is one or more of N-methyl pyrrolidone, N-dimethylformamide, N-dimethylacetamide, dimethyl sulfoxide, m-cresol or gamma-butyrolactone.
According to the preparation method of the polyimide composite film easy to cut, the inorganic filler is any one of calcium carbonate, kaolin, talcum powder, mica, aluminum hydroxide, magnesium hydroxide, pyrophyllite, gypsum, bentonite, sepiolite or attapulgite.
According to the preparation method of the polyimide composite film easy to cut, the inorganic filler is any one of flaky mica, flaky talcum powder or flaky pyrophyllite, and the particle size is 3-5 micrometers.
The polyimide composite film easy to cut is prepared by the method.
Has the beneficial effects that: compared with the prior art, the invention has the advantages that:
compared with the prior art that the polyimide is prepared by blending modified inorganic filler, the method is simple and convenient, can be manufactured in large batch, is more uniform in dispersion, and has stronger binding force.
The existing polyimide film is serrated due to the entanglement of polymer chain segments per se when being torn, and has certain resistance and viscosity when being cut, so that the existing polyimide film is not beneficial to cutting; according to the invention, strong interaction is formed between the oligomer and the inorganic filler, so that the winding of a molecular chain is effectively reduced, and then the oligomer and the inorganic filler are further polymerized to form a composite film; when the composite film is torn, the stress is concentrated in the inorganic filler, the resistance is small during cutting, the cut is neat, and meanwhile, the composite film has lower cost and is easy to manufacture on a large scale.
Drawings
FIG. 1 shows a left and right enlarged view of a polyimide composite film according to the present invention after being automatically torn;
FIG. 2 is a photograph (left) and an enlarged view (right) of the polyimide film prepared in comparative example 1 after tearing;
FIG. 3 is a photograph (left) and an enlarged view (right) of the polyimide composite film prepared in comparative example 2 after tearing;
fig. 4 is a photograph (left) and an enlarged view (right) after the polyimide film prepared in comparative example 3 was torn.
Detailed Description
In order to make the aforementioned objects, features and advantages of the present invention more comprehensible, embodiments accompanying specific embodiments of the present invention are described in detail below.
Example 1
A preparation method of a polyimide composite film easy to cut comprises the following steps:
(1) Preparation of oligomer:
weighing 21.6g of p-phenylenediamine, dissolving the p-phenylenediamine in 262g of N, N-dimethylacetamide, performing ultrasonic dispersion under the stirring condition, adding 44.13g of 3,3',4' -biphenyltetracarboxylic dianhydride, and stirring for 6 hours to obtain an oligomer glue solution, wherein the solid content of the oligomer glue solution is 20wt%;
(2) Coating treatment of inorganic filler:
adding 666g of mica powder Mia powder with Mohs hardness of 2.5, flaky shape and particle size of 4 mu m and 560 g of coupling agent KH 33 into the oligomer glue solution prepared in the step (1), and sanding for 6 hours to obtain uniform slurry with viscosity of about 1000mPa & S;
(3) Preparing a composite glue solution:
weighing 6.03kg of 4,4' -diaminodiphenyl ether in a 100L reaction kettle, adding 53kg of N, N-dimethylacetamide, stirring to dissolve, transferring the slurry prepared in the step (2) to the reaction kettle, emulsifying for 1h, and then adding 6.57kg of pyromellitic dianhydride to perform polycondensation reaction to obtain a composite glue solution; controlling the solid content of the composite glue solution to be 20wt% and the apparent viscosity to be 40000 mPas.S;
(4) Preparing a polyimide film:
and (3) forming the composite glue solution prepared in the step (3) into a film on casting equipment, and then heating and curing, wherein the highest temperature of heating and curing is set at 380 ℃, the length of a drying tunnel is 28m, the speed of the casting equipment is 5m/min, and the time of the whole film drying process is 15min, so that the polyimide composite film PI-S1 is obtained.
Example 2
A polyimide composite film PI-S2 was obtained in the same manner as in example 1 except that the same inorganic filler mica Mia as in example 1 was used and the mass was 1.41kg and the mass of KH560 was 70 g.
Example 3
A polyimide composite film PI-S3 was obtained in the same manner as in example 1 except that the same inorganic filler mica Mia as in example 1 was used, the mass was 3.17kg, and the mass of KH560 was 158 g.
Example 4
(1) Preparing an oligomer;
weighing 86.4g of p-phenylenediamine, dissolving the p-phenylenediamine in 1.04kg of N, N-dimethylacetamide under the condition of stirring, ultrasonically dispersing the p-phenylenediamine, then adding 176.52g of 3,3',4' -biphenyltetracarboxylic dianhydride, and stirring the mixture for 6 hours to obtain an oligomer glue solution, wherein the solid content of the oligomer glue solution is 20wt%;
(2) Coating inorganic filler;
adding 5.40kg of mica powder Mia powder with Mohs hardness of 2.5 and sheet shape and 270g of coupling agent KH560 g into the oligomer glue solution prepared in the step (4-1), and sanding for 6h to obtain uniform slurry with viscosity of about 1000mPa & S;
in the same manner as in example 1 except for the above, a polyimide composite film PI-S4 was obtained.
Example 5
A polyimide composite film PI-S5 was prepared in the same manner as in example 4 except that the same inorganic filler mica Mia as in example 1 was used and the mass was 8.40kg and the mass was 420g in KH560.
Example 6
A polyimide film PI-S6 was obtained in the same manner as in example 4 except that the same inorganic filler mica Mia as in example 1 was used and the mass was 5.40kg and that the mass of KH560 was 270 g.
Example 7
A polyimide film PI-S7 was produced in the same manner as in example 4 except that talc (having a flake-like inorganic filler, a Mohs hardness of 2.5, a particle diameter of 4.3 μm, a mass of 5.40kg, and a KH560 g was used.
Comparative example 1
Weighing 6.00kg of 4,4' -diaminodiphenyl ether and 50kg of N, N-dimethylacetamide (DMAc) in a 100L reaction kettle, emulsifying and stirring for 2h, adding 6.40kg of pyromellitic dianhydride (PMDA) after complete dissolution, and continuously stirring for 12h at room temperature to obtain transparent, homogeneous and viscous polyamide acid (PAA) glue solution. Subsequently, a polyimide film PI-D1 was obtained in the same manner as in example 1.
Comparative example 2
The inorganic filler is changed into granular titanium dioxide TiO with Mohs hardness of 6 and grain diameter of 5.0 mu m 2 In the same manner as in example 3, a polyimide film PI-D2 was produced.
Comparative example 3
Weighing 6.03kg of diamine monomer 4,4' -diaminodiphenyl ether, 3.17kg of flaky mica Mia (Mohs hardness of 2.5 and particle size of 4 mu m) and 158g of KH560 in a 100L reaction kettle, adding 53kg of solvent N, N-dimethylacetamide, stirring and dissolving, transferring the slurry prepared in the step (2) to the reaction kettle, emulsifying for 1h, and then adding 6.57kg of dianhydride monomer pyromellitic dianhydride to perform polycondensation reaction to obtain a composite glue solution; controlling the solid content of the glue solution to be 20wt% and the apparent viscosity to be 40000 mPas.S; film baking was carried out in the same manner as in example 1 to obtain a polyimide film PI-D3.
The test method comprises the following steps:
film cutting resistance test: place the roll-shaped film in the rolling machine, the blade of force sensor is taken in the installation, carries out rolling cutting to the film and handles, and the rolling speed is: and 5m/min, and the resistance value is recorded by the sensor.
Self-tearing morphology: a small opening is drawn in the middle of a film sample strip (100mm 30mm), the film sample strip is torn by hands, the self-tearing morphology of the film is obtained, and the film sample strip is magnified and observed by a quadratic element image measuring instrument.
And (3) testing mechanical properties: the film samples were cut and tested according to the national standard GB/T1040.3 using a universal stretcher from MTS, model E42.
The test results are shown in tables 1 and 2. As can be seen from tables 1 and 2, the incorporation of the inorganic filler in a flake form can increase the modulus while maintaining the tensile strength of the polyimide, and at the same time, exert the "easy-to-cut" effect of the present invention. The polyimide composite film prepared by the mode of sanding of the oligomer, the coupling agent and the inorganic filler has better performance.
TABLE 1 self-tear morphology results for polyimide films
TABLE 2 Performance results for polyimide films
| Sample (I) | Tensile strength/MPa | modulus/GPa | Elongation at break/% |
| PI-D1 | 100 | 2.5 | 22 |
| PI-D2 | 98 | 3.3 | 10 |
| PI-D3 | 99 | 4.0 | 15 |
| PI-S1 | 109 | 2.7 | 15 |
| PI-S2 | 122 | 3.6 | 21 |
| PI-S3 | 107 | 4.1 | 18 |
| PI-S4 | 103 | 5.3 | 15 |
| PI-S5 | 106 | 6.4 | 8 |
| PI-S6 | 102 | 5.1 | 14 |
| PI-S7 | 100 | 4.8 | 18 |
Claims (10)
1. The preparation method of the polyimide composite film easy to cut is characterized by comprising the following steps:
(1) Preparing an oligomer; adding a diamine monomer into a solvent, stirring, emulsifying and dispersing, then adding a dianhydride monomer, and stirring for 6 to 12h to obtain an oligomer glue solution; the dianhydride monomer is added in an amount of 70-90% of the molar weight of the diamine monomer, and the solid content of the oligomer glue solution is 20-40 wt%;
(2) Coating inorganic filler; adding inorganic filler and coupling agent into the oligomer glue solution obtained in the step (1), and performing sand grinding or ball milling for 6 to 12h to obtain uniform slurry; the addition amount of the oligomer glue solution is 5-20 wt% of the inorganic filler, and the addition amount of the coupling agent is 1-10 wt% of the inorganic filler; the Mohs hardness of the inorganic filler is lower than 3, and the particle size is 500nm to 15 mu m;
(3) Preparing a composite glue solution; adding a diamine monomer into a solvent, stirring and dissolving, adding the slurry obtained in the step (2) for emulsification, and then adding a dianhydride monomer for polycondensation reaction to obtain a composite glue solution; the solid content of the composite glue solution is 5-30 wt%, and the apparent viscosity is 5000-300000 mPa.S; step (3), the adding amount of the slurry is controlled to be 10-40 wt% of the inorganic filler in the finished polyimide composite film, and the using ratio of the polymer resin is 60-90 wt%;
(4) Preparing a polyimide composite film: and (4) carrying out tape casting on the composite glue solution obtained in the step (3) to form a film, and then heating and curing to obtain a finished polyimide composite film.
2. The preparation method of the easy-to-cut polyimide composite film according to claim 1, wherein in the step (2), the addition amount of the oligomer glue solution is 8-15 wt% of the mass of the inorganic filler, and the addition amount of the coupling agent is 2-6 wt% of the mass of the inorganic filler; the coupling agent is one or a mixture of more of gamma-aminopropyltriethoxysilane KH550, gamma-glycidoxypropyltrimethoxysilane KH560 or gamma-methacryloxypropyltrimethoxysilane KH 570.
3. The preparation method of the easy-to-cut polyimide composite film as claimed in claim 1, wherein in the step (2), the addition amount of the oligomer glue solution is 10wt% -12 wt% of the mass of the inorganic filler, and the addition amount of the coupling agent is 3wt% -5 wt% of the mass of the inorganic filler.
4. The preparation method of the easy-to-cut polyimide composite film as claimed in claim 1, wherein the solid content of the composite glue solution is 15wt% to 20wt%, and the apparent viscosity is 30000 to 60000 mPa.S.
5. The method for preparing the easy-to-cut polyimide composite film according to claim 1, wherein in the step (3), the addition amount of the slurry is controlled to be 15wt% to 30wt% of the inorganic filler in the finished polyimide composite film, and the addition amount of the polymer resin is controlled to be 70wt% to 85wt%.
6. The method for preparing the easy-to-cut polyimide composite film according to claim 1, wherein in the step (4), the temperature for heating and curing is 200 to 400 ℃, the length of the drying tunnel is 20 to 30m, the speed of a casting device is 2.5 to 10m/min, the time of the whole film drying process is 6 to 24min, and the thickness of the finished polyimide composite film is 5 to 150 μm.
7. <xnotran> 1 , , , ,4,4'- ,4,4' - ,1,3- (4 '- ) ,1,4- (4- ) ,2,2' - ( ) ,4,4'- -2,2' - -1,1'- ,4,4' - ,2,2- [4- (4- ) ] ,2- (4- ) -5- , ,3,3 '- ,4,4' - ,2, 2'- ,4,4- ,4,4' - (3- ) ,4,4'- (4- ) 4,4' - (3- ) ,2,2- [4- (4- ) ] ; </xnotran>
<xnotran> (PMDA), 3,3',4,4' - ,2,3,3 ',4' - ,3,3',4,4 ' - ,4,4' - ,2,3,3 ',4' - ,2,2 ' - (3,4- ) ,1,2,4,5- , -3,4,3',4' - ,4,4' - ,9,9- (3,4- ) ,3,3,4,4- ,4,4' - (4,4 ' - ) - - ; </xnotran>
The solvent is one or more of N-methyl pyrrolidone, N-dimethylformamide, N-dimethylacetamide, dimethyl sulfoxide, m-cresol or gamma-butyrolactone.
8. The method for preparing a polyimide composite film easy to cut according to claim 1, wherein the inorganic filler is any one of calcium carbonate, kaolin, talc, mica, aluminum hydroxide, magnesium hydroxide, pyrophyllite, gypsum, bentonite, sepiolite and attapulgite.
9. The method for preparing a polyimide composite film easy to cut according to claim 1, wherein the inorganic filler is any one of flaky mica, flaky talcum powder or flaky pyrophyllite, and the particle size is 3 to 5 μm.
10. A cuttable polyimide composite film prepared by the method of any one of claims 1 to 9.
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Denomination of invention: A kind of easily cut polyimide composite film and its preparation method Effective date of registration: 20230627 Granted publication date: 20230117 Pledgee: Bank of Jiangsu Limited by Share Ltd. Wuxi Cheng industry sub branch Pledgor: WUXI SHUNXUAN NEW MATERIALS CO.,LTD. Registration number: Y2023980045599 |
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