CN102587217B - Preparation method of polyimide fiber insulating paper - Google Patents
Preparation method of polyimide fiber insulating paper Download PDFInfo
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- CN102587217B CN102587217B CN201210084971.XA CN201210084971A CN102587217B CN 102587217 B CN102587217 B CN 102587217B CN 201210084971 A CN201210084971 A CN 201210084971A CN 102587217 B CN102587217 B CN 102587217B
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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 insulating materials technology of preparing, specifically a kind of preparation method of polyimide fiber insulating paper.This insulating paper is mainly used between the groove of the 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 the equipment such as electrical equipment (generator, transformer etc.), household electrical appliance, electric tool, is also the chief component material of the insulating materials such as laminated product, composite and preimpregnation material.Due to the specific use of insulating paper, require it must possess the characteristic that some are different from other paper kind, mainly comprise mechanical performance, electric property and heat endurance.And because all kinds of electrical equipments use under different environment, as damp and hot, chemical plant (being with mordant chemical reagent), radioactive environment etc., just require insulating paper also to there is good physical and chemical performance and radiation resistance.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 capacity, harsh variation and to improve service life etc. significant conforms.
Polyimide fiber is to prepare a kind of in the high temperature resistant synthetic fiber of insulating paper.Polyimide fiber heat resistance is splendid, 360 ℃ of the load deformation temperature of polypyromelliticimide, and 260 ℃ of long-term serviceability temperatures, under anaerobic, serviceability temperature is 300 ℃, 600 ℃ of heat decomposition temperatures; Weightless approximately 30% after it processes 200h in 400 ℃ of air, under 300 ℃ of nitrogen, process 1000h after intensity decline hardly; Polyimide fiber can the low temperature of resistance to the utmost point, and embrittlement does not occur in the liquid helium of one 269 ℃; Polyimide fiber resistant to high energy radiation is extremely strong, through 1 * 10
10after the fast electron irradiation of rad, its strength retention is still 90%, and after high energy r radiation exposure 8000 times, fibre strength and electrical property are substantially constant; Although there is the polarity gene of some in polyimide fiber, symmetrical configuration and macromolecular main chain are rigidity, have limited the activity of polar group, therefore electrical insulating property is extremely outstanding, dielectric constant is 3.4, and dielectric loss remains on 10
-4level, dielectric strength is 100-300kV/mm, volume resistance 10
17Ω cm; Polyimide fiber thermal coefficient of expansion is little, belongs to 10
-5-10
-7/ ℃ the order of magnitude, and owing to there is no hydrophilic radical in the large molecule of polyimides, water absorption rate is low, so its goods are not yielding under high temperature or high wet condition, has good DIMENSIONAL STABILITY; Polyimide fiber is self-extinguishing, and the rate of being fuming is low, has good fire resistance.
The current 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 is also the routine techniques of preparing insulating paper.The shortcomings such as wet papermaking technology is to take the paper technology that water is medium, and this technology exists production process many, and efficiency is low, and technique is difficult to control, high to equipment requirement, and energy consumption is large.And manufacture paper with pulp in process in wet method, in order to solve dispersed, the good combination problem of fiber, often needing to add the auxiliary agents such as dispersant, technology difficulty is large.At present, the insulating paper product that domestic wet production business produces, the uniformity is poor, is difficult to meet the application requirements aspect high-tech.
US Patent No. 6294049B1 discloses a kind of manufacture method of polyimides paper, its main manufacture process is first polyamic acid solution to be made to polyamic acid fibrid through wet spinning, then by wet papermaking technology, obtain the l Water Paper of polyamic acid, finally by polyimides paper is prepared in chemical imidization or thermal cyclization processing excessively.Polyimides paper prepared by the method only adopts fibrid (fiber is shorter, is approximately 1mm), and the product strength obtaining is not high, and adopts wet papermaking technology, and equipment is complicated, and energy consumption is large.
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, makes it dispersed in water under the effect of pulper, makes pulp.Then adopt wet papermaking technology to make polyimides l Water Paper, finally l Water Paper is processed 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 large, if cut into so short fiber, the loss that will certainly strengthen the energy, and wet papermaking can not meet the requirement of environmental protection, can bring certain pollution to environment.
US Patent No. 20070084575A1 has announced a kind of method of producing composite sheet, it is first dispersed in polyimide fiber in the suspension of polytetrafluorethylepowder powder, and add additive as polyimide resin or epoxy resin, after through wet papermaking machine, obtain l Water Paper, finally by super-dry, heating pressurized treatments, obtained the composite sheet of polyimides and polytetrafluoroethylene (PTFE).Although it is strong that polytetrafluorethylepowder powder has corrosion resistance, the advantages such as good heat resistance and electrical property are good, but it also has a lot of shortcomings, as poor in radiation resistance, viscosity not, linear expansion coefficient is large etc., because polytetrafluorethylepowder powder has not viscosity, be added in polyimide fiber, can cause the paper of preparing easily to produce surperficial defectiveness, the problems such as layering, and the linear expansion coefficient of polytetrafluorethylepowder powder is larger, can there is along with the variation of temperature very erratic variation, in the process of hot rolling, material will produce larger distortion, make product size less stable, quality is not good.
Summary of the invention
For the deficiencies in the 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 technique is simple, controls easily, and easy to operate, energy consumption is low, and products obtained therefrom is high temperature resistant, and insulating properties is good, good flame resistance, resistance to chemical attack, easily industrializing implementation.
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 polyimides fibre web; Then first this fibre web at room temperature be impregnated in to 10-30min in polyamic acid binder solution, reinforce this fibre web, after the mangle that is 100-300% through pick-up rate, fibre web is sent into dry processing in baking oven, finally by mould pressing process, make polyimide fiber insulating paper; The length of described polyimide fiber is 20-78mm, and fiber number is 0.7-8.0dtex; Described polyamic acid binder solution is by forming with the polyamic acid resin of component and the solvent requirement that by volume concentration is 0.3-30% configuration with polyimide fiber, two kinds of adopting a kind of or arbitrary proportion in DMF, DMAc and NMP to mix of described solvent; Described baking temperature is 40-130 ℃, and be 0.5-6h drying time; Described mould pressing process is used moulding press, and parameter designing is: molding temperature 150-350 ℃, 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 from polyimide fiber component, and technique is simple, controls easily, and energy consumption is low, pollution-free, meets 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
Below in conjunction with embodiment, further introduce the present invention:
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 → be dried → be molded into paper; Specifically: adopt polyimide fiber as raw material, pass through conventional shredding, combing and to 90 ° of cross lappings, obtain polyimides fibre web in length and breadth, then first adopt chemical adhesion method by fibre web at room temperature impregnated in the polyamic acid binder solution of fiber with component in, reinforce fibre web, after mangle, fibre web is sent into dry processing in baking oven, then through mould pressing process, make polyimide fiber insulating paper
The raw material that preparation method of the present invention adopts is only single polyimide fiber (abbreviation fiber), and design fibre length is 20-78mm, and fiber number is 0.7-8.0dtex.
Shredding described in preparation method of the present invention, carding technique itself are prior art.Shredding and carding equipment that conventional enterprise has all can be realized this technique.In preparation method of the present invention, fibrous raw material is only polyimide fiber, and raw material is single, therefore only need to use opener to carry out shredding, has reduced the mixed processes in conventional nonwoven fabric preparation method, so technological process shortening, Energy Intensity Reduction, cost savings.Particularly, prior art patent (as aforementioned US6294049B1, JP2003-96698, US20070084575A1 etc.) all adopts wet-laying method to prepare fibre web, compare with the Wet technique that prior art adopts, the carding method technique that the present invention adopts is simple, energy consumption is low, and do not need to add the auxiliary agents such as polytetrafluorethylepowder powder, epoxy resin, pollution-free, cost is low.
In preparation method of the present invention, the fibre web going out due to shredding, combing is very thin, if adopt conventional lapping mode, fibre web larger than very to brute force in length and breadth, is unfavorable for that the brute force of product is balanced.Fiber after combing of the present invention needs in length and breadth to the lapping technique of 90 ° of cross lappings, can make polyimides fibre web.Adopt in length and breadth to 90 ° of cross lapping techniques, can make to distribute in all angles direction of fiber in fibre web more even, reduced in length and breadth to brute force ratio, guarantee that product is powerful balanced.Described is applicant's formerly patented technology (referring to ZL201010267320.5) in length and breadth to 90 ° of cross lapping techniques.
Because polyimide fiber does not have fusing point, as direct employing mould pressing process, between fiber and fiber, cohesive force is inadequate, and the product making has larger defect at aspects such as intensity, uniformities, so preparation method's special design of the present invention has adopted chemical impregnation adhesion technique.This process using is by the method for combing gained fibre web dipping polyamic acid adhesive, cementation between reinforcing fibre, and the polyamic acid adhesive using 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 making is very high, at aspects such as uniformities, also makes moderate progress.In preparation method of the present invention, to fibre web chemical impregnation adhesive, be also important operation, whether the performance indications such as intensity that are related to the insulating paper preparing meet the requirements.Chemical impregnation adhesion technique need to configure certain density polyamic acid adhesive, if binder concn is excessive, while flooding, adhesive is difficult for infiltration in fibre web, produce fibre web and flood irregular phenomenon, and if binder concn is too small, after drying, the applied amount of adhesive is less for fibre web, can make to bond between fiber insufficient, the low strength of insulating paper.Through experimental study, the volumetric concentration of described polyamic acid adhesive is designed to 0.3-30%; Another technological parameter of chemical impregnation adhesion technique is pick-up rate; If pick-up rate is too small, in fibre web, binder content is less, between fiber, bond insufficient, the insulating paper brute force obtaining is lower, and easily occurs the phenomenon of layering, and if pick-up rate is excessive, in fibre web, binder content is larger, and adhesive is not easy dispersed in insulating paper, and the uniformity of the insulating paper making is bad, therefore to determine suitable pick-up rate, so that the performance of the insulating paper of preparing reaches optimum state.Research shows, pick-up rate is that 100-300% effect is better.Obviously, chemical impregnation adhesion technique also needs suitable dip time, and long or too short dip time all can affect the effect of chemical impregnation adhesion technique, and through experimental study, described dip time is designed to 10-30min.
The compound method of described polyamic acid adhesive is, polyamic acid resin and the solvent proportional arrangement that by volume concentration is 0.3-30% are formed, described solvent adopts DMF(N, dinethylformamide), DMAc(N, N-dimethylacetylamide) and NMP(N-methyl pyrrolidone) in two kinds of mixing of a kind of or arbitrary proportion.
The dipping method technique that preparation method of the present invention adopts is simple, control easily, the polyamic acid adhesive adopting is and the polyimide precursor of polyimide fiber with component, be that adhesive is identical with the component of fiber, therefore compare with the preparation method of the polyimide fiber insulating paper of prior art, the indexs such as the electric property of the insulating paper that this preparation method makes, heat resistance, cold resistance are all more excellent.
In preparation method of the present invention, drying process is fibre web to be put into baking oven be dried, to remove all solvent waters.Dry is to make adhesive that partly solidified process occur, and can improve the intensity of fibre web after being dried, and baking temperature is 40-130 ℃, and be 0.5-6h drying time.
Mould pressing process described in preparation method of the present invention is one of critical process.The object of mold pressing is that adhesive is occurred is completely curing, to improve the indexs such as intensity, tearability, breakdown strength of insulating paper, and makes 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.Embodiment molding apparatus adopts moulding press, and parameter designing is: molding temperature 150-350 ℃, molding pressure 2-25MPa, clamp time 5-90min.
Adopt the preparation method of polyimide fiber insulating paper of the present invention can directly make polyimide fiber insulating paper.After measured, the thickness of insulating paper of the present invention is that 0.05-0.9mm(records according to standard GB/T/T 24218.2-2009), grammes per square metre is 40-300g/m
2(according to standard GB/T/T 24218.1-2009, recording), vertical, horizontal tensile strength is respectively 120-280N/15mm and 100-250N/15mm(vertical, horizontal tensile strength records according to standard GB/T/T453-2002), dielectric constant 1.09-1.38(records according to Unite States Standard ASTMD150), dielectric loss angle tangent 0.001-0.006(records according to standard GB/T/T1409-2006), resistivity is 1.82-2.95 * 10
8Ω m(records according to Unite States Standard ASTMD150), air dielectric intensity 8.1-19.7kV/mm, insulating oil dielectric intensity 10.4-23.5kV/mm(air dielectric intensity and insulating oil dielectric intensity record according to standard GB/T/T 1408.1-2006); 250 ℃ of horizontal percent thermal shrinkages are 0.05-0.26%, and longitudinally percent thermal shrinkage is that 0.23-0.61%(is horizontal, longitudinally percent thermal shrinkage records according to standard GB/T 12027-2004); General insulating materials is 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 processed after 5min in the liquid nitrogen of-196 ℃, measure its vertical, horizontal creasy recovery angle and only lose respectively 1.8-4.2% and 0.5-1.5%, 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 material is not easy by thermal breakdown.Test shows, insulating paper of the present invention belongs to highest ranking H level in 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, although the polyimide insulative paper that exists various preparation methods to make does not all clearly show about the property indices 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 embodiments of the invention below.These specific embodiments, only for further narration the present invention, do not limit the claim protection domain of the present patent application.
embodiment 1
(1) net processed: selecting length is the polyimide fiber that 20mm, fiber number are 0.7dtex, through conventional shredding, combing, and adopts in length and breadth to 90 ° of cross lappings, makes polyimides fibre web;
(2) chemical adhesion and drying technique: polyamic acid resin is dissolved in 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%; Finally by the wet fibre web making dry 1.5h in the baking oven of 110 ℃;
(3) compression molding: the fibre web after drying is used moulding press compression molding, obtains product insulating paper; 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, air dielectric intensity 19.7kV/mm, insulating oil dielectric intensity 23.5kV/mm; 250 ℃ of horizontal percent thermal shrinkages are 0.13%, and longitudinally percent thermal shrinkage is 0.4%; At-196 ℃, process after 5min, its vertical, horizontal creasy recovery angle only loses respectively 1.8% and 0.5%.
embodiment 2
(1) net processed: selecting length is the polyimide fiber that 78mm, fiber number are 1.5dtex, through conventional shredding, combing, and adopts in length and breadth to 90 ° of cross lappings, makes polyimides fibre web;
(2) chemical adhesion and drying technique: polyamic acid resin is dissolved in 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%; Finally by the wet fibre web making dry 6h in the baking oven of 40 ℃;
(3) compression molding: the fibre web after drying is used moulding press compression molding, obtains product insulating paper; 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, air dielectric intensity 12.5kV/mm, insulating oil dielectric intensity 18.6kV/mm; 250 ℃ of horizontal percent thermal shrinkages are 0.18%, and longitudinally percent thermal shrinkage is 0.54%; At-196 ℃, process after 5min, its vertical, horizontal creasy recovery angle only loses respectively 2.7% and 0.8%.
embodiment 3
(1) net processed: selecting length is the polyimide fiber that 45mm, fiber number are 2.0dtex, through conventional shredding, combing, and adopts in length and breadth to 90 ° of cross lappings, makes polyimides fibre web;
(2) chemical adhesion and drying technique: polyamic acid resin is dissolved in 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%, finally by the wet fibre web making dry 2.2h in the baking oven of 90 ℃;
(3) compression molding: the fibre web after drying is used moulding press compression molding, obtains product insulating paper; 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, air dielectric intensity 13.4kV/mm, insulating oil dielectric intensity 19.2kV/mm; 250 ℃ of horizontal percent thermal shrinkages are 0.26%, and longitudinally percent thermal shrinkage is 0.61%; At-196 ℃, process after 5min, its vertical, horizontal creasy recovery angle only loses respectively 3.5% and 1.5%.
embodiment 4
(1) net processed: selecting length is the polyimide fiber that 35mm, fiber number are 8.0dtex, through conventional shredding, combing, and adopts in length and breadth to 90 ° of cross lappings, makes polyimides fibre web;
(2) chemical adhesion and drying technique: polyamic acid resin is dissolved in to DMF and DMAc and take volume ratio in the mixed solvent of 1:2:2 preparation, 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%, finally by the wet fibre web making dry 0.5h in the baking oven of 130 ℃;
(3) compression molding: the fibre web after drying is used moulding press compression molding, obtains product insulating paper; 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, air dielectric intensity 18.3kV/mm, insulating oil dielectric intensity 21.2kV/mm; 250 ℃ of horizontal percent thermal shrinkages are 0.18%, and longitudinally percent thermal shrinkage is 0.35%; At-196 ℃, process after 5min, its vertical, horizontal creasy recovery angle only loses respectively 2.2% and 1.3%.
embodiment 5
(1) net processed: selecting length is the polyimide fiber that 60mm, fiber number are 4.5dtex, through conventional shredding, combing, and adopts in length and breadth to 90 ° of cross lappings, makes polyimides fibre web;
(2) chemical adhesion and drying technique: polyamic acid resin is dissolved in to DMAc and NMP and take volume ratio in the mixed solvent of 2:10:13 ratio preparation, 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%, finally by the wet fibre web making dry 3.5h in the baking oven of 70 ℃;
(3) compression molding: the fibre web after drying is used moulding press compression molding, obtains product insulating paper; 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, air dielectric intensity 18.7kV/mm, insulating oil dielectric intensity 23.1kV/mm; 250 ℃ of horizontal percent thermal shrinkages are 0.08%, and longitudinally percent thermal shrinkage is 0.26%; At-196 ℃, process after 5min, its vertical, horizontal creasy recovery angle only loses respectively 4.2% and 1.4%.
Claims (4)
1. a preparation method for 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 polyimides fibre web; Then first this fibre web at room temperature be impregnated in to 10-30min in polyamic acid binder solution, reinforce this fibre web, after the mangle that is 100-300% through pick-up rate, fibre web is sent into dry processing in baking oven, finally by mould pressing process, make polyimide fiber insulating paper; The length of described polyimide fiber is 20-78mm, and fiber number is 0.7-8.0dtex; Described polyamic acid binder solution is by forming with the polyamic acid resin of component and the solvent requirement that by volume concentration is 0.3-30% configuration with polyimide fiber, two kinds of adopting a kind of or arbitrary proportion in DMF, DMAc and NMP to mix of described solvent; Described baking temperature is 40-130 ℃, and be 0.5-6h drying time; Described mould pressing process is used moulding press, and parameter designing is: molding temperature 150-350 ℃, 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 polyimide fiber insulating paper described in claim 1.
3. polyimide fiber insulating paper according to claim 2, the thickness that it is characterized in that described 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, air dielectric intensity 8.1-19.7kV/mm, insulating oil dielectric intensity 10.4-23.5kV/mm; 250 ℃ of horizontal percent thermal shrinkages are 0.05-0.26%, and longitudinally percent thermal shrinkage is 0.23-0.61%: described insulating paper is processed after 5min at-196 ℃, and its vertical, horizontal creasy recovery angle loses respectively 1.8-4.2% and 0.5-1.5%.
4. a polyimide fiber insulating paper claimed in claim 3, is characterized in that this insulating paper is H level, for High-Frequency Special Transformer, high voltage high frequency transformer or hydraulic generator machine equipment.
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| CN102747634B (en) * | 2012-07-27 | 2014-11-19 | 陕西科技大学 | Method for preparing modified polyimide fiber papers |
| 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 |
| CN107723826B (en) * | 2017-11-03 | 2020-01-14 | 东华大学 | Method for continuously producing colored polyimide fibers by two-step method |
| 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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| DE69320697T2 (en) * | 1992-06-09 | 1999-02-18 | Unitika Ltd | Polyimide paper, polyimide composite paper and process for making these products |
| JP2003096698A (en) * | 2001-09-27 | 2003-04-03 | Unitika Ltd | Heat-resistant insulating paper sheet and method for producing the same |
| JP2005133260A (en) * | 2003-10-31 | 2005-05-26 | Unitika Ltd | Composite paper-like material |
| EP2363429A1 (en) * | 2006-03-10 | 2011-09-07 | Goodrich Corporation | Low density lightining strike protection for use in airplanes |
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