CN109385089B - Polyamide acid resin synthesis method combining strictly equimolar monomers with compensation feeding - Google Patents
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- C08G73/10—Polyimides; Polyester-imides; Polyamide-imides; Polyamide acids or similar polyimide precursors
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Abstract
The invention discloses a polyamide acid resin synthesis method by strictly equimolar monomer combination compensation feeding. The method adopts a strict equimolar monomer combination compensation feeding mode, simultaneously, through extrusion coating, longitudinal and transverse biaxial orientation stretching orientation and repeated cold and hot circulation treatment, the polyimide film is prepared, the prepared polyimide film has high mechanical strength, low shrinkage and good heat resistance, and can meet the common requirements of the field of electric power and electrical appliance insulation and winding electromagnetic wires and the high-end requirement of flexible circuit preparation.
Description
Technical Field
The invention belongs to the technical field of polyimide film preparation, and particularly relates to a polyamide acid resin synthesis method by strictly equimolar monomer combination compensation feeding.
Background
At present, the main application field of the polyimide film in China is electric power and electrical appliance insulation and electromagnetic wire wrapping. The polyimide film is a key insulating material of electric power and electrical appliances, is widely applied to the manufacture of power transmission and distribution equipment, wind power generation equipment, variable frequency motors, high-speed traction motors, high-voltage transformers and the like, and plays a unique role in the currently common electrical insulating film. Since the last 90 years, high-performance polyimide film materials have become key materials for microelectronic fabrication and packaging, and are widely applied to the fabrication of very large scale integrated circuits, flexible packaging substrates, flexible connecting strip lines and the like. The polyimide film can not be separated from high-speed rails with the speed of 300 kilometers per hour to electronic products such as notebook computers, mobile phones, cameras, video cameras and the like with tiny miniaturization. According to statistics, the annual demand of polyimide films in China in the last year exceeds 2800 tons, and products of foreign companies such as America and the like account for 80 percent of market share in China. The production technology of the high-performance polyimide film is mainly mastered in developed countries such as America and the like. Standard polyimide films from dupont, usa have been kept at a high monopoly price of about 1000 yuan/kg for nearly 10 years.
The adhesive tape prepared by coating the fluorinated ethylene propylene emulsion on one surface or two surfaces of the polyimide film serving as the base material can be wrapped on a bare copper wire, has good heat resistance, thin and uniform insulating layer thickness and good sealing property, and improves the moisture resistance and the electrical property of the wire.
However, the existing polyimide film has poor flexibility, and the physical properties and sealing properties are reduced under high temperature conditions, so that the polyimide film is not suitable for preparing high-end products such as flexible circuit boards.
Disclosure of Invention
The invention aims to provide a polyamide acid resin synthesis method with strictly equimolar monomer combined compensation feeding.
A polyamide acid resin synthesis method of strictly equimolar monomer combined compensation feeding is carried out according to the following steps:
(1) mixing aromatic diamine and tetracarboxylic dianhydride in equal molar number, adding catalyst triethylamine, heating to 30-80 ℃ to initiate polymerization reaction, and stirring for 2-24h to prepare slurry;
(2) adding carbon nanotubes into the slurry, and uniformly mixing to prepare composite slurry;
(3) sending the composite slurry prepared in the step (2) into an extrusion coating machine, coating polyimide resin liquid onto a steel belt through an extrusion die head, and controlling the thickness of the film through a gap at the outlet of the electronic control die head;
(4) and (3) sending the polyimide film subjected to extrusion coating film formation in the step (3) into an imidization furnace, carrying out imidization treatment, simultaneously carrying out longitudinal and transverse biaxial oriented stretching orientation, and finally carrying out repeated cold-heat cycle treatment to obtain a final product.
The aromatic diamine is m-phenylenediamine, p-phenylenediamine, 3,3 '-dimethylbenzidine, 2, 5-diaminotoluene, 4, 4' -diaminobenzophenone or 2, 4-diamino-6-chlorotoluene.
The tetracarboxylic dianhydride is 3,3 ', 4, 4' -benzophenonetetracarboxylic dianhydride, pyromellitic dianhydride, 3,3 ', 4, 4' -biphenyltetracarboxylic dianhydride, 2, 2 ', 3, 3' -biphenyltetracarboxylic dianhydride, 1, 4, 5, 8-naphthalenetetracarboxylic dianhydride, 1, 2,5, 6-naphthalenetetracarboxylic dianhydride, phenanthrene-1, 8, 9, 10-tetracarboxylic dianhydride or benzene-1, 2, 3, 4-tetracarboxylic dianhydride.
The thickness of the film in the step (3) is 15-25 um.
The longitudinal stretching magnification of the longitudinal and transverse biaxial oriented stretching orientation is 1.8-2.8, and the transverse stretching magnification is 5.0-9.2.
The time interval of the repeated cold-hot circulation treatment is 6-12s, the cold circulation temperature is 30-50 ℃, the hot circulation temperature is 155-185 ℃, and the circulation frequency is 20-50.
Triethylamine accounting for 0.1 to 0.5 percent of the total weight of the mixture is added in the step (1).
The invention has the beneficial effects that: the invention adopts a strict equimolar monomer combined compensation feeding mode to prepare the polyimide film, and the prepared polyimide film has high mechanical strength, low shrinkage rate and good heat resistance, and can meet the common requirements in the fields of electric and electric appliance insulation and electromagnetic wire wrapping and the high-end requirement of flexible circuit preparation.
Detailed Description
The present invention is further illustrated by the following specific examples.
Example 1
A polyamide acid resin synthesis method of strictly equimolar monomer combined compensation feeding is carried out according to the following steps:
(1) mixing m-phenylenediamine and 3,3 ', 4, 4' -benzophenone tetracarboxylic dianhydride in equal molar numbers, adding 0.1% of catalyst triethylamine, heating to 50 ℃ to initiate polymerization reaction, and stirring for 12 hours to prepare slurry;
(2) adding 1% of carbon nano tubes into the slurry, and uniformly mixing to prepare composite slurry;
(3) sending the composite slurry prepared in the step (2) into an extrusion coating machine, coating polyimide resin liquid onto a steel belt through an extrusion die head, and controlling the thickness of the film through a gap at the outlet of the electronic control die head; the thickness of the film was 18 um;
(4) sending the polyimide film subjected to extrusion coating film formation in the step (3) into an imidization furnace, carrying out imidization treatment, simultaneously carrying out longitudinal and transverse biaxial oriented stretching orientation, and finally carrying out repeated cold-heat cycle treatment to obtain a final product; the longitudinal stretching multiplying power of the longitudinal and transverse biaxial oriented stretching orientation is 2.2, and the transverse stretching multiplying power is 6.2; the time interval of the repeated cold-hot circulation treatment is 8s, the cold circulation temperature is 40 ℃, the hot circulation temperature is 175 ℃, and the circulation frequency is 30 times.
Example 2
A polyamide acid resin synthesis method of strictly equimolar monomer combined compensation feeding is carried out according to the following steps:
(1) mixing 3, 3' -dimethylbenzidine and pyromellitic dianhydride in equal molar number, adding 0.2% of catalyst triethylamine, heating to 30 ℃ to initiate polymerization reaction, and stirring for 8 hours to prepare slurry;
(2) adding 1% of carbon nano tubes into the slurry, and uniformly mixing to prepare composite slurry;
(3) sending the composite slurry prepared in the step (2) into an extrusion coating machine, coating polyimide resin liquid onto a steel belt through an extrusion die head, and controlling the thickness of the film through a gap at the outlet of the electronic control die head; the thickness of the film was 15 um;
(4) sending the polyimide film subjected to extrusion coating film formation in the step (3) into an imidization furnace, carrying out imidization treatment, simultaneously carrying out longitudinal and transverse biaxial oriented stretching orientation, and finally carrying out repeated cold-heat cycle treatment to obtain a final product; the longitudinal stretching multiplying power of the longitudinal and transverse biaxial oriented stretching orientation is 1.8, and the transverse stretching multiplying power is 5.0; the time interval of the repeated cold-hot circulation treatment is 6s, the cold circulation temperature is 30 ℃, the hot circulation temperature is 155 ℃, and the circulation frequency is 20 times.
Example 3
A polyamide acid resin synthesis method of strictly equimolar monomer combined compensation feeding is carried out according to the following steps:
(1) mixing 2, 5-diaminotoluene and phenanthrene-1, 8, 9, 10-tetracarboxylic dianhydride in equal molar number, adding 0.5% of catalyst triethylamine, heating to 80 ℃ to initiate polymerization reaction, and stirring for 24 hours to prepare slurry;
(2) adding 1% of carbon nano tubes into the slurry, and uniformly mixing to prepare composite slurry;
(3) sending the composite slurry prepared in the step (2) into an extrusion coating machine, coating polyimide resin liquid onto a steel belt through an extrusion die head, and controlling the thickness of the film through a gap at the outlet of the electronic control die head; the thickness of the film was 25 um;
(4) sending the polyimide film subjected to extrusion coating film formation in the step (3) into an imidization furnace, carrying out imidization treatment, simultaneously carrying out longitudinal and transverse biaxial oriented stretching orientation, and finally carrying out repeated cold-heat cycle treatment to obtain a final product; the longitudinal stretching multiplying power of the longitudinal and transverse biaxial oriented stretching orientation is 2.8, and the transverse stretching multiplying power is 9.2; the time interval of the repeated cold-hot circulation treatment is 12s, the cold circulation temperature is 50 ℃, the hot circulation temperature is 185 ℃, and the circulation frequency is 50 times.
Example 4
A polyamide acid resin synthesis method of strictly equimolar monomer combined compensation feeding is carried out according to the following steps:
(1) mixing m-phenylenediamine and 3,3 ', 4, 4' -benzophenone tetracarboxylic dianhydride in equal molar numbers, adding 0.1% of catalyst triethylamine, heating to 50 ℃ to initiate polymerization reaction, and stirring for 12 hours to prepare slurry;
(2) adding 1% of carbon nano tube and 1% of 4- [ trans-4- (trans-4-propylcyclohexyl) cyclohexyl ] toluene into the slurry, and uniformly mixing to prepare composite slurry;
(3) sending the composite slurry prepared in the step (2) into an extrusion coating machine, coating polyimide resin liquid onto a steel belt through an extrusion die head, and controlling the thickness of the film through a gap at the outlet of the electronic control die head; the thickness of the film was 18 um;
(4) sending the polyimide film subjected to extrusion coating film formation in the step (3) into an imidization furnace, carrying out imidization treatment, simultaneously carrying out longitudinal and transverse biaxial oriented stretching orientation, and finally carrying out repeated cold-heat cycle treatment to obtain a final product; the longitudinal stretching multiplying power of the longitudinal and transverse biaxial oriented stretching orientation is 2.2, and the transverse stretching multiplying power is 6.2; the time interval of the repeated cold-hot circulation treatment is 8s, the cold circulation temperature is 40 ℃, the hot circulation temperature is 175 ℃, and the circulation frequency is 30 times.
Example 5
A polyamide acid resin synthesis method of strictly equimolar monomer combined compensation feeding is carried out according to the following steps:
(1) mixing m-phenylenediamine and 3,3 ', 4, 4' -benzophenone tetracarboxylic dianhydride in equal molar numbers, adding 0.1% of catalyst triethylamine, heating to 50 ℃ to initiate polymerization reaction, and stirring for 12 hours to prepare slurry;
(2) adding 1% of carbon nano tube and 1% of Sr Be Eu into the slurry2O5Uniformly mixing the crystal powder to prepare composite slurry;
(3) sending the composite slurry prepared in the step (2) into an extrusion coating machine, coating polyimide resin liquid onto a steel belt through an extrusion die head, and controlling the thickness of the film through a gap at the outlet of the electronic control die head; the thickness of the film was 18 um;
(4) sending the polyimide film subjected to extrusion coating film formation in the step (3) into an imidization furnace, carrying out imidization treatment, simultaneously carrying out longitudinal and transverse biaxial oriented stretching orientation, and finally carrying out repeated cold-heat cycle treatment to obtain a final product; the longitudinal stretching multiplying power of the longitudinal and transverse biaxial oriented stretching orientation is 2.2, and the transverse stretching multiplying power is 6.2; the time interval of the repeated cold-hot circulation treatment is 8s, the cold circulation temperature is 40 ℃, the hot circulation temperature is 175 ℃, and the circulation frequency is 30 times.
Example 6
A polyamide acid resin synthesis method of strictly equimolar monomer combined compensation feeding is carried out according to the following steps:
(1) mixing m-phenylenediamine and 3,3 ', 4, 4' -benzophenone tetracarboxylic dianhydride in equal molar numbers, adding 0.1% of catalyst triethylamine, heating to 50 ℃ to initiate polymerization reaction, and stirring for 12 hours to prepare slurry;
(2) to the slurry was added 1% carbon nanotubes, 1% K (Al Ge)3O8) Uniformly mixing the crystal powder to prepare composite slurry;
(3) sending the composite slurry prepared in the step (2) into an extrusion coating machine, coating polyimide resin liquid onto a steel belt through an extrusion die head, and controlling the thickness of the film through a gap at the outlet of the electronic control die head; the thickness of the film was 18 um;
(4) sending the polyimide film subjected to extrusion coating film formation in the step (3) into an imidization furnace, carrying out imidization treatment, simultaneously carrying out longitudinal and transverse biaxial oriented stretching orientation, and finally carrying out repeated cold-heat cycle treatment to obtain a final product; the longitudinal stretching multiplying power of the longitudinal and transverse biaxial oriented stretching orientation is 2.2, and the transverse stretching multiplying power is 6.2; the time interval of the repeated cold-hot circulation treatment is 8s, the cold circulation temperature is 40 ℃, the hot circulation temperature is 175 ℃, and the circulation frequency is 30 times.
Experimental example:
with reference to the requirements of the international standard IEC 60674-3-4/6: 1993: shrinkage rate of not more than 0.06% at 150 deg.C and 400 deg.C, and volume resistivity of not less than 1012Omega, m, surface resistivity is not less than 1014Omega. The shrinkage at 150 ℃ and 400 ℃, the volume resistivity and the surface resistivity of examples 1 to 6 of the present invention were measured, and the results are shown in tables 1 and 2.
TABLE 1
Note: represents P <0.05 compared to the example 1 group.
As can be seen from Table 1, the shrinkage rates at 400 ℃ of examples 1 to 6 are less than 0.06% at 150 ℃ and satisfy the requirements of the international standard IEC 60674-3-4/6: 1993; the 150 ℃ and 400 ℃ shrinkage rates of the samples of the examples 4 to 5 are obviously better than those of the sample of the example 1, and the effect is better.
TABLE 2
Note: represents P <0.05 compared to the example 1 group.
As can be seen from Table 2, examples 1-6 have volume resistivities greater than 1012M, surface resistivity greater than 1014Omega, meets the requirements of international standard IEC 60674-3-4/6: 1993; the volume resistivity and the surface resistivity of the samples 4 to 5 are obviously better than those of the sample 1, and the effect is better.
Claims (1)
1. A polyimide film synthesis method combining strictly equimolar monomers with compensation feeding is carried out according to the following steps:
(1) mixing m-phenylenediamine and 3,3 ', 4, 4' -benzophenone tetracarboxylic dianhydride in equal molar numbers, adding 0.1% of catalyst triethylamine, heating to 50 ℃ to initiate polymerization reaction, and stirring for 12 hours to prepare slurry;
(2) adding 1% of carbon nano tube and 1% of 4- [ trans-4- (trans-4-propylcyclohexyl) cyclohexyl ] toluene into the slurry, and uniformly mixing to prepare composite slurry;
(3) sending the composite slurry prepared in the step (2) into an extrusion coating machine, coating polyimide resin liquid onto a steel belt through an extrusion die head, and controlling the thickness of the film through a gap at the outlet of the electronic control die head; the thickness of the film was 18 um;
(4) sending the polyimide film subjected to extrusion coating film formation in the step (3) into an imidization furnace, carrying out imidization treatment, simultaneously carrying out longitudinal and transverse biaxial oriented stretching orientation, and finally carrying out repeated cold-heat cycle treatment to obtain a final product; the longitudinal stretching multiplying power of the longitudinal and transverse biaxial oriented stretching orientation is 2.2, and the transverse stretching multiplying power is 6.2; the time interval of the repeated cold-hot circulation treatment is 8s, the cold circulation temperature is 40 ℃, the hot circulation temperature is 175 ℃, and the circulation frequency is 30 times.
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| 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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| 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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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 |