CN102587217A - Preparation method of polyimide fiber insulating paper - Google Patents
Preparation method of polyimide fiber insulating paper Download PDFInfo
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- CN102587217A CN102587217A CN201210084971XA CN201210084971A CN102587217A CN 102587217 A CN102587217 A CN 102587217A CN 201210084971X A CN201210084971X A CN 201210084971XA CN 201210084971 A CN201210084971 A CN 201210084971A CN 102587217 A CN102587217 A CN 102587217A
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Abstract
The invention discloses a preparation method of polyimide fiber insulating paper. The preparation method comprises the following steps of: adopting a polyimide fiber with a length of 20-78 mm and a fiber number of 0.7-8.0 dtex as a raw material, and obtaining a polyimide fiber net through conventional opening, carding and lapping; and then, impregnating the fiber net into a polyamic acid adhesive solution for 10-30 minutes, passing the fiber net through a mangle with a mangle expression of 100-300%, and then, drying the fiber net, and finally, preparing the polyimide fiber insulating paper through a mould pressing process, wherein the adhesive solution is prepared from polyamic acid resin with the same components as the polyimide fiber and a solvent according to a requirement that the volume concentration is 0.3-30%; the solvent is selected from one or two of DMF (dimethyl formamide), DMAc (dimethyl acetamide ) and NMP (N-methyl pyrrolidone) mixed in any proportion; the drying temperature is 40-130 DEG C and the drying time is 0.5-6 hours; and the mould pressing process is that the mould pressing temperature is 150-350 DEG C, the mould pressing pressure is 2-25 MPa, and the mould pressing time is 5-90 minutes.
Description
Technical field
The present invention relates to the insulating materials technology of preparing, specifically is a kind of preparation method of polyimide fiber insulating paper.This insulating paper is mainly used between the groove of equipment such as high frequency special transformer, high voltage high frequency transformer, hydrogenerator and the insulation of interlayer.
Background technology
Insulating paper is widely used in the insulating materials of equipment such as electrical equipment (generator, transformer etc.), household electrical appliance, electric tool, also is the main composition material of insulating materials such as laminated product, composite and preimpregnation material.Because the specific use of insulating paper requires it must possess the characteristic that some are different from other paper kind, mainly comprises mechanical performance, electric property and heat endurance.And,, just require insulating paper also to have better physical chemical property and radiation resistance like damp and hot, chemical plant (having corrosive chemical reagent), radioactive environment etc. because all kinds of electrical equipments use under different environment.In recent years, the exploitation of high temperature resistant synthetic-fibre insulating paper has obtained faster development, its to various electrical equipments realize miniaturization, high capacities, harsh variation and to improve service life etc. significant conforms.
Polyimide fiber be the preparation insulating paper high temperature resistant synthetic fiber in a kind of.The polyimide fiber heat resistance is splendid, 360 ℃ of the load deformation temperature of equal benzene type polyimides, and 260 ℃ of long-term serviceability temperatures, serviceability temperature is 300 ℃ under the anaerobic, 600 ℃ of heat decomposition temperatures; It handles behind the 200h weightless about 30% in 400 ℃ of air, and intensity descends hardly behind processing 1000h 300 ℃ of nitrogen under; Polyimide fiber can the low temperature of anti-the utmost point, and embrittlement does not take place in one 269 ℃ liquid helium; Polyimide fiber resistant to high energy radiation property is extremely strong, through 1 * 10
10Behind the fast electron irradiation of rad, its strength retention still is 90%, and after high energy r radiation exposure 8000 times, fibre strength and electrical property are constant basically; Though there is the polarity gene of some in the polyimide fiber, symmetrical configuration and macromolecular main chain are rigidity, have limited the activity of polar group, so electrical insulating property is extremely outstanding, dielectric constant is 3.4, and dielectric loss remains on 10
-4Level, dielectric strength are 100-300kV/mm, volume resistance 10
17Ω cm; The polyimide fiber thermal coefficient of expansion is little, belongs to 10
-5-10
-7/ ℃ the order of magnitude, and owing to do not have hydrophilic radical in the big molecule of polyimides, water absorption rate is low, so its goods are not yielding under high temperature still is high wet condition, has good DIMENSIONAL STABILITY; Polyimide fiber is a self-extinguishing, and the rate of being fuming is low, has good flame retardant property.
The present both at home and abroad preparation method of insulating paper adopts the moulding of manufacturing paper with pulp of wet papermaking technology more, and it also is the routine techniques of preparation insulating paper.Shortcomings such as the wet papermaking technology is to be the paper technology of medium with water, and this technology exists production process many, and efficient is low, and difficult technique is with control, and is high to equipment requirements, and energy consumption is big.And in wet method is manufactured paper with pulp process,, often need add auxiliary agents such as dispersant for even dispersion, the good combination problem that solves fiber, technology difficulty is big.At present, the insulating paper product that domestic wet production merchant produces, the uniformity is relatively poor, is difficult to satisfy the application requirements aspect high-tech.
U.S. Pat 6294049B1 discloses a kind of manufacturing approach of polyimides paper; Its main manufacture process is earlier polyamic acid solution to be made the polyamic acid fibrid through wet spinning; Obtain the l Water Paper of polyamic acid then through the wet papermaking technology, go out polyimides paper through chemical cyclisation or thermal cyclization Processing of Preparation at last.The polyimides paper of this method preparation only adopts fibrid (fiber is shorter, is approximately 1mm), and the product strength that obtains is not high, and adopts the wet papermaking technology, complex equipments, and energy consumption is big.
Japan patent of invention 2003-96698 has announced a kind of method of producing high temperature insulation paper, is about to the staple fibre that polyimide fiber cuts into 3-12mm, and it is evenly disperseed in water, processes pulp.Adopt the wet papermaking technology to make the polyimides l Water Paper then, at last l Water Paper is handled through heating (heating-up temperature is between the glass transition temperature and fusing point of fiber), pressurization (pressure is that 0.05-10Mpa is advisable), just obtained polyimides paper.But polyimide fiber intensity, rigidity are all very big, if it is cut into the fiber of weak point like this, will certainly strengthen the loss of the energy, and wet papermaking can not satisfy environmental protection requirement, can bring certain pollution to environment.
U.S. Pat 20070084575A1 has then announced a kind of method of producing composite sheet; It is dispersed in polyimide fiber in the suspension of polytetrafluorethylepowder powder earlier; And adding additive such as polyimide resin or epoxy resin; After obtain l Water Paper through the wet papermaking machine, handle through super-dry, heating and pressurizing at last, obtained the composite sheet of polyimides and polytetrafluoroethylene (PTFE).Advantages such as corrosion resistance is strong though polytetrafluorethylepowder powder has, good heat resistance and electrical property are good, it also has a lot of shortcomings, and is relatively poor like radiation resistance, viscosity, linear expansion coefficient are big etc.; Because of polytetrafluorethylepowder powder has not viscosity; It is added in the polyimide fiber, can cause the paper of preparing to be prone to produce problems such as surperficial defectiveness, layering, and the linear expansion coefficient of polytetrafluorethylepowder powder is bigger; Very erratic variation can take place along with variation of temperature; Material will produce bigger distortion in the process of hot rolling, make the product size less stable, and quality is not good.
Summary of the invention
To the deficiency of prior art, the technical problem that quasi-solution of the present invention is determined is that a kind of preparation method of polyimide fiber insulating paper is provided.This preparation method's technology is simple, and control is easy, and easy to operate, energy consumption is low, and products obtained therefrom is high temperature resistant, and insulating properties is good, good flame resistance, and resistance to chemical attack, easy for industrialized is implemented.
The technical scheme that the present invention solve the technical problem is; Design a kind of preparation method of polyimide fiber insulating paper; This preparation method adopts polyimide fiber as raw material, through conventional shredding, combing with in length and breadth to 90 ° of cross lappings, obtains the polyimides fibre web; Earlier at room temperature impregnated in 10-30min in the polyamic acid binder solution to this fibre web then; Reinforce this fibre web, be the mangle of 100-300% through pick-up rate after, fibre web is sent into dried in the baking oven; After mould pressing process promptly makes the polyimide fiber insulating paper; The length of said polyimide fiber is 20-78mm, and fiber number is 0.7-8.0dtex; Said polyamic acid binder solution by with polyimide fiber with the polyamic acid resin of component and solvent by volume concentration be that the requirement configuration of 0.3-30% forms, two kinds of adopting a kind of or arbitrary proportion among DMF, DMAc and the NMP to mix of said solvent; Said baking temperature is 40-130 ℃, and be 0.5-6h drying time; Said mould pressing process uses moulding press, and parameter designing is: molding temperature 150-350 ℃, and molding pressure 2-25MPa, clamp time 5-90min.
Compared with prior art, the raw material that polyimide fiber insulating paper preparation method of the present invention adopts is single, does not add other material different with the polyimide fiber component, and technology is simple, and control is easy, and energy consumption is low, and is pollution-free, meets the modern production requirement; Do not use special or new equipment, the conventional equipment of relevant enterprise is applicable preparation method of the present invention, and industrializing implementation is easy; Preparation method's gained polyimide fiber insulating paper properties of product of the present invention are good, and insulating properties is excellent, good flame resistance, and resistance to chemical attack, steady quality, and cost is low.
The specific embodiment
Further introduce the present invention below in conjunction with embodiment:
The preparation method (abbreviation preparation method) of the polyimide fiber insulating paper (abbreviation insulating paper) of the present invention design, its technological process is: polyimide fiber → shredding carding → chemical impregnation is bonding → dry → be molded into paper; Be specifically: adopt polyimide fiber as raw material; Through conventional shredding, combing with obtain the polyimides fibre web to 90 ° of cross lappings in length and breadth, adopt earlier then the chemical adhesion method with fibre web at room temperature impregnated in the polyamic acid binder solution of fiber with component in, reinforce fibre web; Behind the mangle; Fibre web is sent into dried in the baking oven,, promptly make the polyimide fiber insulating paper again through mould pressing process
The raw material that preparation method of the present invention adopts is merely single polyimide fiber (abbreviation fiber), and the design fibre length is 20-78mm, and fiber number is 0.7-8.0dtex.
The described shredding of preparation method of the present invention, carding technology itself are prior art.Shredding and carding equipment that conventional enterprise is had all can be realized this technology.In preparation method of the present invention, fibrous raw material is merely polyimide fiber, and raw material is single, therefore only needs to use opener to carry out shredding and gets final product, and has reduced the mixed processes among the conventional nonwoven fabric preparation method, so the technological process shortening, and energy consumption reduces, cost savings.Particularly; Prior art patent (like aforementioned US6294049B1, JP2003-96698, US20070084575A1 etc.) all adopts the wet-laying method to prepare fibre web, compares with the Wet technique that prior art adopts, and the carding method technology that the present invention adopts is simple; Energy consumption is low; And need not add auxiliary agents such as polytetrafluorethylepowder powder, epoxy resin, pollution-free, cost is low.
Among the preparation method of the present invention, because the fibre web that shredding, combing go out is very thin, if adopt conventional lapping mode, fibre web big than very to brute force in length and breadth is unfavorable for the powerful equilibrium of product.Fiber after the combing of the present invention needs can make the polyimides fibre web in length and breadth to the lapping technology of 90 ° of cross lappings.Adopt in length and breadth to 90 ° of cross lapping technologies, can make more even distribution on all angles direction of fiber in fibre web, reduced in length and breadth, guarantee that product is powerful balanced to the brute force ratio.Said is applicant's patented technology formerly (referring to ZL201010267320.5) in length and breadth to 90 ° of cross lapping technologies.
Because polyimide fiber does not have fusing point; Like direct employing mould pressing process; Cohesive force is not enough between fiber and the fiber, and the product that makes has big defective at aspects such as intensity, uniformities, so preparation method of the present invention designs especially and adopted the chemical impregnation adhesion technique.This process using is with the method for combing gained fibre web dipping polyamic acid adhesive; Cementation between the reinforcing fibre; And the polyamic acid adhesive that uses obtains after thermal cyclization reaction is polyimides; Therefore adopt this adhesive all can not exert an influence to the heat resistance of product, electric property etc., the insulating paper intensity that makes is very high, also makes moderate progress at aspects such as uniformities.Among the preparation method of the present invention, also be important operation to fibre web chemical impregnation adhesive, whether the performance indications such as intensity that are related to the insulating paper for preparing meet the requirements.The chemical impregnation adhesion technique need dispose certain density polyamic acid adhesive, if binder concn is excessive, adhesive is difficult for infiltration when then flooding in fibre web; Produce the irregular phenomenon of fibre web dipping; And if binder concn is too small, fibre web is after drying, and the applied amount of adhesive is less; Can make that bonding is insufficient between the fiber, the intensity of insulating paper is on the low side.Through experimental study, the volumetric concentration of said polyamic acid adhesive is designed to 0.3-30%; Another technological parameter of chemical impregnation adhesion technique is a pick-up rate; If pick-up rate is too small, then binder content is less in the fibre web, and bonding is insufficient between the fiber; The insulating paper brute force that obtains is lower, and occurs the phenomenon of layering easily, and if pick-up rate is excessive; Then binder content is bigger in the fibre web, and adhesive is not easy even dispersion in insulating paper, and the uniformity of the insulating paper that makes is bad; Therefore to confirm suitable pick-up rate, so that the performance of the insulating paper of preparing reaches optimum state.Research shows that pick-up rate is that the 100-300% effect is better.Obviously, the chemical impregnation adhesion technique also needs suitable dip time, and long or too short dip time all can influence the effect of chemical impregnation adhesion technique, and through experimental study, described dip time is designed to 10-30min.
The compound method of said polyamic acid adhesive is; With polyamic acid resin and solvent by volume concentration be that the proportional arrangement of 0.3-30% forms; Said solvent adopts DMF (N; Dinethylformamide), two kinds of the mixing of a kind of or arbitrary proportion among DMAc (DMAC N,N) and the NMP (N-Methyl pyrrolidone).
The dipping method technology that preparation method of the present invention adopts is simple; Control easily; The polyamic acid adhesive that is adopted is and the polyimide precursor of polyimide fiber with component; Therefore be that adhesive is identical with the component of fiber, compare with the preparation method of the polyimide fiber insulating paper of prior art that indexs such as the electric property of the insulating paper that this preparation method makes, heat resistance, cold resistance are all more excellent.
Among the preparation method of the present invention, drying process is fibre web to be put into baking oven carry out drying, to remove all solvent waters.Drying is to make adhesive that partly solidified process take place, and can improve the intensity of fibre web after the drying, and baking temperature is 40-130 ℃, and be 0.5-6h drying time.
The described mould pressing process of preparation method of the present invention is one of critical process.The purpose of mold pressing is to make adhesive take place to solidify fully, with indexs such as the intensity that improves insulating paper, tearability, breakdown strengths, and makes the insulating paper surface more smooth, meets its instructions for use.The molding temperature that preparation method's mould pressing process of the present invention adopts depends on the solidification temperature of polyamic acid adhesive.The embodiment molding apparatus adopts moulding press, and parameter designing is: molding temperature 150-350 ℃, and molding pressure 2-25MPa, clamp time 5-90min.
Adopt the preparation method of polyimide fiber insulating paper of the present invention can directly make the polyimide fiber insulating paper.Through measuring, the thickness of insulating paper of the present invention is 0.05-0.9mm (recording according to standard GB/T 24218.2-2009), and grammes per square metre is 40-300g/m
2(recording) according to standard GB/T 24218.1-2009; The vertical, horizontal tensile strength is respectively 120-280N/15mm and 100-250N/15mm (the vertical, horizontal tensile strength records according to standard GB/T453-2002); Dielectric constant 1.09-1.38 (ASTMD150 records according to Unite States Standard); Dielectric loss angle tangent 0.001-0.006 (recording according to standard GB/T1409-2006), resistivity are 1.82-2.95 * 10
8Ω m (ASTMD150 records according to Unite States Standard); Dielectric strength 8.1-19.7kV/mm in the air, dielectric strength 10.4-23.5kV/mm in the insulating oil (in the air in dielectric strength and the insulating oil dielectric strength record) according to standard GB/T 1408.1-2006; 250 ℃ of horizontal percent thermal shrinkages are 0.05-0.26%, and vertically percent thermal shrinkage is 0.23-0.61% (horizontal, vertical percent thermal shrinkage records according to standard GB/T 12027-2004); General insulating materials is the meeting embrittlement in liquid nitrogen; Lose its insulating properties; Therefore the present invention has tested the resistance to low temperature of insulating paper in liquid nitrogen especially: the insulating paper of embodiment is handled 5min in-196 ℃ liquid nitrogen after; Measure its vertical, horizontal creasy recovery angle and only lose 1.8-4.2% and 0.5-1.5% respectively, show that the resistance to low temperature of insulating paper of the present invention is fabulous.Polyimide fiber has lower dielectric constant, can make the Electric Field Distribution between insulation and cooling medium more even, and dielectric loss angle tangent is lower, and then material is not easy by thermal breakdown.Test shows; Insulating paper of the present invention belongs to highest ranking H level in the insulating paper; Can be used for doing between the groove in the equipment such as high frequency special transformer, high voltage high frequency transformer or hydrogenerator and the insulating materials of interlayer, and be suitable in the special occasions such as high temperature resistant, corrosion-resistant, radiation hardness.In the scope of applicant retrieval, though the polyimide insulative paper that exists various preparation methods to make does not all clearly show about each item performance indications prior art of polyimide insulative paper, and the purposes of polyimide insulative paper is not described yet.
The present invention does not address part and is applicable to prior art.
Provide specific embodiment of the present invention below.These specific embodiments only are used for further narrating the present invention, do not limit the claim protection domain of application of the present invention.
Embodiment 1
(1) system net: selecting length for use is that 20mm, fiber number are the polyimide fiber of 0.7dtex, through conventional shredding, combing, and adopts in length and breadth to 90 ° of cross lappings, makes the polyimides fibre web;
(2) chemical adhesion and drying technology: polyamic acid resin is dissolved in the solvent DMF; Stir 30min, make volumetric concentration and be 30% polyamic acid binder solution, then fibre web is immersed in the binder solution of joining; Dipping 30min, pick-up rate is 100%; Wet fibre web dry 1.5h in 110 ℃ baking oven that will make at last;
(3) compression molding: the fibre web behind the drying uses the moulding press compression molding, promptly obtains the product insulating paper; The die press technology for forming parameter is: 150 ℃ of molding temperatures, molding pressure 25Mpa, clamp time 90min.
Through check, this insulating paper grammes per square metre 48g/m
2, thickness 0.05mm, machine direction tensile strength 120N/15mm, cross direction tensile strength 100N/15mm, dielectric constant 1.17, dielectric loss angle tangent 0.002, resistivity is 2.1 * 10
8Ω m, dielectric strength 19.7kV/mm in the air, dielectric strength 23.5kV/mm in the insulating oil; 250 ℃ of horizontal percent thermal shrinkages are 0.13%, and vertically percent thermal shrinkage is 0.4%; After handling 5min under-196 ℃, its vertical, horizontal creasy recovery angle only loses 1.8% and 0.5% respectively.
Embodiment 2
(1) system net: selecting length for use is that 78mm, fiber number are the polyimide fiber of 1.5dtex, through conventional shredding, combing, and adopts in length and breadth to 90 ° of cross lappings, makes the polyimides fibre web;
(2) chemical adhesion and drying technology: polyamic acid resin is dissolved among the solvent DMAc; Stir 30min, make volumetric concentration and be 0.3% polyamic acid binder solution, then fibre web is immersed in the binder solution of joining; Dipping 25min, pick-up rate is 300%; Wet fibre web dry 6h in 40 ℃ baking oven that will make at last;
(3) compression molding: the fibre web behind the drying uses the moulding press compression molding, promptly obtains the product insulating paper; The die press technology for forming parameter is: 350 ℃ of molding temperatures, molding pressure 2Mpa, clamp time 30min.
Through check, this insulating paper grammes per square metre 190g/m
2, thickness 0.18mm, machine direction tensile strength 143N/15mm, cross direction tensile strength 121N/15mm, dielectric constant 1.09, dielectric loss angle tangent 0.003, resistivity is 2.03 * 10
8Ω m, dielectric strength 12.5kV/mm in the air, dielectric strength 18.6kV/mm in the insulating oil; 250 ℃ of horizontal percent thermal shrinkages are 0.18%, and vertically percent thermal shrinkage is 0.54%; After handling 5min under-196 ℃, its vertical, horizontal creasy recovery angle only loses 2.7% and 0.8% respectively.
Embodiment 3
(1) system net: selecting length for use is that 45mm, fiber number are the polyimide fiber of 2.0dtex, through conventional shredding, combing, and adopts in length and breadth to 90 ° of cross lappings, makes the polyimides fibre web;
(2) chemical adhesion and drying technology: polyamic acid resin is dissolved among the solvent NMP; Stir 30min; Make volumetric concentration and be 12% polyamic acid binder solution, then fibre web is immersed in the binder solution of joining, dipping 10min; Pick-up rate is 135%, wet fibre web dry 2.2h in 90 ℃ baking oven that will make at last;
(3) compression molding: the fibre web behind the drying uses the moulding press compression molding, promptly obtains the product insulating paper; The die press technology for forming parameter is: 220 ℃ of molding temperatures, molding pressure 20Mpa, clamp time 50min.
Through check, this insulating paper grammes per square metre 100g/m
2, thickness 0.15mm, machine direction tensile strength 158N/15mm, cross direction tensile strength 136N/15mm, dielectric constant 1.27, dielectric loss angle tangent 0.001, resistivity is 2.06 * 10
8Ω m, dielectric strength 13.4kV/mm in the air, dielectric strength 19.2kV/mm in the insulating oil; 250 ℃ of horizontal percent thermal shrinkages are 0.26%, and vertically percent thermal shrinkage is 0.61%; After handling 5min under-196 ℃, its vertical, horizontal creasy recovery angle only loses 3.5% and 1.5% respectively.
Embodiment 4
(1) system net: selecting length for use is that 35mm, fiber number are the polyimide fiber of 8.0dtex, through conventional shredding, combing, and adopts in length and breadth to 90 ° of cross lappings, makes the polyimides fibre web;
(2) chemical adhesion and drying technology: polyamic acid resin is dissolved in the mixed solvent that DMF and DMAc are the 1:2:2 preparation with the volume ratio; Stir 30min; Make volumetric concentration and be 20% polyamic acid binder solution, then fibre web is immersed in the binder solution of joining, dipping 22min; Pick-up rate is 260%, wet fibre web dry 0.5h in 130 ℃ baking oven that will make at last;
(3) compression molding: the fibre web behind the drying uses the moulding press compression molding, promptly obtains the product insulating paper; The die press technology for forming parameter is: 280 ℃ of molding temperatures, molding pressure 12Mpa, clamp time 20min.
Through check, this insulating paper grammes per square metre 240g/m
2, thickness 0.25mm, machine direction tensile strength 228N/15mm, cross direction tensile strength 205N/15mm, dielectric constant 1.31, dielectric loss angle tangent 0.004, resistivity is 2.26 * 10
8Ω m, dielectric strength 18.3kV/mm in the air, dielectric strength 21.2kV/mm in the insulating oil; 250 ℃ of horizontal percent thermal shrinkages are 0.18%, and vertically percent thermal shrinkage is 0.35%; After handling 5min under-196 ℃, its vertical, horizontal creasy recovery angle only loses 2.2% and 1.3% respectively.
Embodiment 5
(1) system net: selecting length for use is that 60mm, fiber number are the polyimide fiber of 4.5dtex, through conventional shredding, combing, and adopts in length and breadth to 90 ° of cross lappings, makes the polyimides fibre web;
(2) chemical adhesion and drying technology: polyamic acid resin is dissolved in DMAc and NMP with the volume ratio in the mixed solvent for the preparation of 2:10:13 ratio; Stir 30min; Make volumetric concentration and be 8% polyamic acid binder solution, then fibre web is immersed in the binder solution of joining, dipping 18min; Pick-up rate is 200%, wet fibre web dry 3.5h in 70 ℃ baking oven that will make at last;
(3) compression molding: the fibre web behind the drying uses the moulding press compression molding, promptly obtains the product insulating paper; The die press technology for forming parameter is: 250 ℃ of molding temperatures, molding pressure 17Mpa, clamp time 5min.
Through check, this insulating paper grammes per square metre 280g/m
2, thickness 0.30mm, machine direction tensile strength 195N/15mm, cross direction tensile strength 169N/15mm, dielectric constant 1.25, dielectric loss angle tangent 0.003, resistivity is 2.56 * 10
8Ω m, dielectric strength 18.7kV/mm in the air, dielectric strength 23.1kV/mm in the insulating oil; 250 ℃ of horizontal percent thermal shrinkages are 0.08%, and vertically percent thermal shrinkage is 0.26%; After handling 5min under-196 ℃, its vertical, horizontal creasy recovery angle only loses 4.2% and 1.4% respectively.
Claims (4)
1. the preparation method of a polyimide fiber insulating paper, this preparation method adopts polyimide fiber as raw material, through conventional shredding, combing with in length and breadth to 90 ° of cross lappings, obtains the polyimides fibre web; Earlier at room temperature impregnated in 10-30min in the polyamic acid binder solution to this fibre web then; Reinforce this fibre web, be the mangle of 100-300% through pick-up rate after, fibre web is sent into dried in the baking oven; After mould pressing process promptly makes the polyimide fiber insulating paper; The length of said polyimide fiber is 20-78mm, and fiber number is 0.7-8.0dtex; Said polyamic acid binder solution by with polyimide fiber with the polyamic acid resin of component and solvent by volume concentration be that the requirement configuration of 0.3-30% forms, two kinds of adopting a kind of or arbitrary proportion among DMF, DMAc and the NMP to mix of said solvent; Said baking temperature is 40-130 ℃, and be 0.5-6h drying time; Said mould pressing process uses moulding press, and parameter designing is: molding temperature 150-350 ℃, and molding pressure 2-25MPa, clamp time 5-90min.
2. a polyimide fiber insulating paper is characterized in that this polyimide fiber insulating paper is directly made by the preparation method of the said polyimide fiber insulating paper of claim 1.
3. polyimide fiber insulating paper according to claim 2, the thickness that it is characterized in that said insulating paper is 0.05-0.9mm, grammes per square metre is 40-300g/m
2, machine direction tensile strength 120-280N/15mm, cross direction tensile strength 100-250N/15mm, dielectric constant 1.09-1.38, dielectric loss angle tangent 0.001-0.006, resistivity is 1.82-2.95 * 10
8Ω m, dielectric strength 8.1-19.7kV/mm in the air, dielectric strength 10.4-23.5kV/mm in the insulating oil; 250 ℃ of horizontal percent thermal shrinkages are 0.05-0.26%, and vertically percent thermal shrinkage is 0.23-0.61%: after handling 5min under-196 ℃, its vertical, horizontal creasy recovery angle loses 1.8-4.2% and 0.5-1.5% respectively with said insulating paper.
4. the described polyimide fiber insulating paper of claim 3 is characterized in that this insulating paper is the H level, is used for high frequency special transformer, high voltage high frequency transformer or hydraulic generator machine equipment.
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102747634A (en) * | 2012-07-27 | 2012-10-24 | 陕西科技大学 | Method for preparing modified polyimide fiber papers |
| CN102926270A (en) * | 2012-10-09 | 2013-02-13 | 陕西科技大学 | Method for preparing polyimide fiber paper |
| CN103495310A (en) * | 2013-09-11 | 2014-01-08 | 昆山市万丰制衣有限责任公司 | Finishing process of pyrohydrolysis-resistant polyimide filtering material |
| CN107142777A (en) * | 2017-06-20 | 2017-09-08 | 长春高琦聚酰亚胺材料有限公司 | A kind of composite polyimide material and preparation method thereof |
| CN107190566A (en) * | 2017-04-27 | 2017-09-22 | 广东粤特变压器有限公司 | A kind of new heat modification insulating paper preparation method based on nano modification Kapton |
| CN107723826A (en) * | 2017-11-03 | 2018-02-23 | 东华大学 | A kind of method that two-step method continuous production prepares coloured polyimide fiber |
| CN110158346A (en) * | 2019-05-31 | 2019-08-23 | 连云港市工业投资集团有限公司 | A kind of polyimide fiber paper based insulation material and preparation method thereof |
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| CN102747634A (en) * | 2012-07-27 | 2012-10-24 | 陕西科技大学 | Method for preparing modified polyimide fiber papers |
| CN102747634B (en) * | 2012-07-27 | 2014-11-19 | 陕西科技大学 | Method for preparing modified polyimide fiber papers |
| CN102926270A (en) * | 2012-10-09 | 2013-02-13 | 陕西科技大学 | Method for preparing polyimide fiber paper |
| CN102926270B (en) * | 2012-10-09 | 2015-06-03 | 陕西科技大学 | Method for preparing polyimide fiber paper |
| CN103495310A (en) * | 2013-09-11 | 2014-01-08 | 昆山市万丰制衣有限责任公司 | Finishing process of pyrohydrolysis-resistant polyimide filtering material |
| CN107190566A (en) * | 2017-04-27 | 2017-09-22 | 广东粤特变压器有限公司 | A kind of new heat modification insulating paper preparation method based on nano modification Kapton |
| CN107142777A (en) * | 2017-06-20 | 2017-09-08 | 长春高琦聚酰亚胺材料有限公司 | A kind of composite polyimide material and preparation method thereof |
| CN107723826A (en) * | 2017-11-03 | 2018-02-23 | 东华大学 | A kind of method that two-step method continuous production prepares coloured polyimide fiber |
| CN107723826B (en) * | 2017-11-03 | 2020-01-14 | 东华大学 | Method for continuously producing colored polyimide fibers by two-step method |
| CN110158346A (en) * | 2019-05-31 | 2019-08-23 | 连云港市工业投资集团有限公司 | A kind of polyimide fiber paper based insulation material and preparation method thereof |
| CN110158346B (en) * | 2019-05-31 | 2021-10-22 | 连云港市工业投资集团有限公司 | Polyimide fiber paper-based insulating material and preparation method thereof |
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