CN104631200A - Polyimide fiber paper with potassium titanate whiskers, and preparation method of polyimide fiber paper - Google Patents
Polyimide fiber paper with potassium titanate whiskers, and preparation method of polyimide fiber paper Download PDFInfo
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- CN104631200A CN104631200A CN201510044226.6A CN201510044226A CN104631200A CN 104631200 A CN104631200 A CN 104631200A CN 201510044226 A CN201510044226 A CN 201510044226A CN 104631200 A CN104631200 A CN 104631200A
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- potassium titanate
- crystal whisker
- titanate crystal
- polyimide fiber
- pulp suspension
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- 239000000835 fiber Substances 0.000 title claims abstract description 185
- 229920001721 polyimide Polymers 0.000 title claims abstract description 118
- 239000004642 Polyimide Substances 0.000 title claims abstract description 117
- NJLLQSBAHIKGKF-UHFFFAOYSA-N dipotassium dioxido(oxo)titanium Chemical compound [K+].[K+].[O-][Ti]([O-])=O NJLLQSBAHIKGKF-UHFFFAOYSA-N 0.000 title claims abstract description 117
- 238000002360 preparation method Methods 0.000 title claims abstract description 19
- 239000006185 dispersion Substances 0.000 claims abstract description 39
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 claims abstract description 35
- 229910000077 silane Inorganic materials 0.000 claims abstract description 35
- 229920003235 aromatic polyamide Polymers 0.000 claims abstract description 21
- 239000013078 crystal Substances 0.000 claims description 113
- 239000000725 suspension Substances 0.000 claims description 108
- 230000004048 modification Effects 0.000 claims description 65
- 238000012986 modification Methods 0.000 claims description 65
- 238000000034 method Methods 0.000 claims description 50
- 238000001035 drying Methods 0.000 claims description 26
- 229920006231 aramid fiber Polymers 0.000 claims description 17
- 206010061592 cardiac fibrillation Diseases 0.000 claims description 16
- 230000002600 fibrillogenic effect Effects 0.000 claims description 16
- 238000007731 hot pressing Methods 0.000 claims description 13
- 239000000203 mixture Substances 0.000 claims description 13
- 238000007493 shaping process Methods 0.000 claims description 13
- 238000000527 sonication Methods 0.000 claims description 13
- 210000000988 bone and bone Anatomy 0.000 claims description 11
- 238000009210 therapy by ultrasound Methods 0.000 claims description 11
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical group [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 claims description 2
- 239000007788 liquid Substances 0.000 claims description 2
- 239000011591 potassium Substances 0.000 claims description 2
- 229910052700 potassium Inorganic materials 0.000 claims description 2
- 239000000463 material Substances 0.000 abstract description 19
- 230000000694 effects Effects 0.000 abstract description 16
- 238000001914 filtration Methods 0.000 abstract description 6
- 229920000297 Rayon Polymers 0.000 abstract description 3
- 239000011810 insulating material Substances 0.000 abstract description 3
- 238000001556 precipitation Methods 0.000 abstract description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 abstract description 3
- 238000005260 corrosion Methods 0.000 abstract description 2
- 230000007797 corrosion Effects 0.000 abstract description 2
- 230000003471 anti-radiation Effects 0.000 abstract 1
- 239000011248 coating agent Substances 0.000 abstract 1
- 238000000576 coating method Methods 0.000 abstract 1
- 230000008878 coupling Effects 0.000 abstract 1
- 238000010168 coupling process Methods 0.000 abstract 1
- 238000005859 coupling reaction Methods 0.000 abstract 1
- 229920005575 poly(amic acid) Polymers 0.000 description 11
- 230000005855 radiation Effects 0.000 description 6
- 230000001413 cellular effect Effects 0.000 description 4
- 239000012774 insulation material Substances 0.000 description 4
- 238000005253 cladding Methods 0.000 description 3
- 239000011347 resin Substances 0.000 description 3
- 229920005989 resin Polymers 0.000 description 3
- 238000009987 spinning Methods 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- 229920000742 Cotton Polymers 0.000 description 2
- 239000012736 aqueous medium Substances 0.000 description 2
- 238000010009 beating Methods 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 229910052739 hydrogen Inorganic materials 0.000 description 2
- 239000001257 hydrogen Substances 0.000 description 2
- 238000002161 passivation Methods 0.000 description 2
- 229920000049 Carbon (fiber) Polymers 0.000 description 1
- 241000826860 Trapezium Species 0.000 description 1
- 238000005299 abrasion Methods 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 238000013459 approach Methods 0.000 description 1
- 125000003118 aryl group Chemical group 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000004917 carbon fiber Substances 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 239000004035 construction material Substances 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000007598 dipping method Methods 0.000 description 1
- 239000003063 flame retardant Substances 0.000 description 1
- 239000003365 glass fiber Substances 0.000 description 1
- 239000003779 heat-resistant material Substances 0.000 description 1
- 230000007062 hydrolysis Effects 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
- 230000003301 hydrolyzing effect Effects 0.000 description 1
- 238000009413 insulation Methods 0.000 description 1
- 238000010297 mechanical methods and process Methods 0.000 description 1
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- 238000005192 partition Methods 0.000 description 1
- 125000005543 phthalimide group Chemical group 0.000 description 1
- 239000009719 polyimide resin Substances 0.000 description 1
- 230000001376 precipitating effect Effects 0.000 description 1
- 230000001681 protective effect Effects 0.000 description 1
- 239000002002 slurry Substances 0.000 description 1
- 229920002994 synthetic fiber Polymers 0.000 description 1
- 239000012209 synthetic fiber Substances 0.000 description 1
- 238000004804 winding Methods 0.000 description 1
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Abstract
The invention discloses polyimide fiber paper with potassium titanate whiskers, and a preparation method of the polyimide fiber paper. Polyimide fibers which are easy to flocculated and difficult to disperse are dispersed through ultrasonic waves, so that the dispersion effect of the polyimide fiber paper in water can be improved; the potassium titanate whiskers are modified by adding silane coupling and have the characteristics of excellent mechanical performance, corrosion resistance, heat-insulating property, high electrical insulating property and the like, so that the strength performance of the polyimide fiber paper can be improved; by taking para-aramid fiber pulp fibers or para-aramid precipitation fibers with large specific surface areas and high surface activity as viscose fibers, a fiber-whisker tiny coating body is formed, so that the interfacial bonding strength of the polyimide fiber paper can be enhanced; the fiber hybrid effect is generated by the polyimide fibers, the potassium titanate whiskers and the para-aramid fiber pulp fibers or the para-aramid precipitation fibers, so that the comprehensive properties of the polyimide fiber paper can be improved, the polyimide fibers can be relatively well applied to a high temperature-insulating material, a filtering material, a high-temperature-insulating anti-radiation material and a honeycomb material.
Description
Technical field
The invention belongs to material and field of papermaking, be specifically related to a kind of polyimide fiber paper adding potassium titanate crystal whisker and preparation method thereof.
Background technology
Polyimides (Polyimide) fiber, being called for short PI fiber, is a kind of high-performance synthetic fiber, is prepared from mainly through high temperature imidizate after polyamic acid solution spinning or by polyimide solution spinning or the happy and harmonious spinning excessively of resin.Polyimide molecule due to its aromatic ring structure density large, have again phthalimide structure, therefore it not only has the characteristic of high-strength and high-modulus simultaneously, but also has high temperature resistant, resistance to chemical attack, the superior performance such as fire-retardant.Compared with the Kelvlar-49 fiber that polyimide fiber and traditional representational du pont company of high-strength and high-modulus amount most develop, polyimide fiber has higher strength and modulus, higher thermo oxidative stability, higher elastic modelling quantity, lower water absorption rate, higher anti-flammability, higher hydrolytic resistance and higher radiation resistance.Therefore, polyimide fiber and polyimide fiber paper sill have very wide application prospect in fields such as high temperature insulating material, Aero-Space and high-performance electronic equipment.Polyimide fiber paper can be used as high-temperature insulation material, filtering material, high temperature resistant radiation resistance material and cellular material.High-temperature insulation material can be used for transformer, motor coil winding, alternate, turn-to-turn line terminal insulating materials; Filtering material can be used for the wideband filtering material of aircraft, guided missile, satellite, can as radar paper cap, radio recognition equipment wave transparent window etc.; High temperature resistant radiation resistance material can be used for the heat resistant material etc. of the heat-barrier material of engine, spark plug, the thermally protective materials such as high temperature resistant, radiation flexible pipe; Cellular material can be used for special construction material, as wing, cabin door liner plate, floor, partition wall etc.
Aramid fiber is in " trapezium structure ", have very high strength and modulus by chemical bond linkage between fiber vertical element, horizontal then linked by hydrogen bond, therefore its Anisotropy characteristic is fairly obvious, so pulp fibers can be obtained by fibrillation, be conducive to paper sheet formation.But, the character of polyimide fiber is very stable, surface passivation, and polyimide fiber is due to higher strength modulus and the higher rigidity of strand, even if seminar's early-stage Study finds also can not produce fibrillation phenomenon through overground making beating process, therefore cannot obtain by precipitation method or Mechanical Method the pulp shape or precipitating shape polyimide fiber that surface-activity is high, specific area is large.
Therefore, the through engineering approaches preparation of polyimide fiber paper is also faced with certain tackling problems in key technologies difficult problem, on the one hand poly-, the difficult dispersion of easily wadding a quilt with cotton of polyimides long fiber causes paper-forming evenness poor, and another aspect lacks Performance Match and surface-activity is high, specific area is large " viscose fibre " causes body paper intensity difference with it.This is difficult to play completely with regard to making the very excellent performance of polyimide fiber, limits its application in field, middle and high end.Application number is the preparation method that the patent of invention of 201210084971.X discloses a kind of polyimide fiber insulating paper, impregnated in polyamic acid solution by polyimides fibre web will be obtained through conventional shredding, combing and lapping, then obtain polyimide fiber insulating paper by the process of high temperature imidizate; Application number be 201210334745.2 patent of invention disclose the preparation method of polyimide fiber paper, utilize polyamic acid fiber to obtain polyamic acid fibrous paper by wet papermaking and obtain polyimide fiber paper by high temperature imidizate again; Application number be 201210380828.5 patent of invention disclose a kind of preparation method of polyimide fiber paper, obtain polyamic acid fibrous paper by utilizing polyamic acid fiber by wet papermaking to impregnated in polyimide resin solution, then obtain polyimide fiber paper by the process of high temperature imidizate; Application number be 201210264309.2 patent of invention disclose a kind of preparation method of modified polyimide fibrous paper, polyimide fiber through aqueous slkali modification is manufactured paper with pulp into polyimide fiber body paper by wet-forming technique, then through polyamic acid solution dipping and imidizate obtain modified polyimide fibrous paper.Being not difficult to find, the patent of invention of several representative polyimides paper described above, is all utilize polyamic acid fiber or polyamic acid solution at high temperature and pressure imidizate to occur thus obtained polyimides paper.Certain defect can be there is in this mode, and the first, polyamic acid fiber itself easily decomposes; The second, the moisture produced in the process of imidizate easily causes hole in polyimide fiber; 3rd, if the condition controls such as temperature, pressure are improper, there will be imidizate incomplete, strand is due to height-oriented, and molecule activity is restricted, and makes the polyamic acid fiber of not yet imidizate be difficult to continue cyclisation, causes molecular mass to decline; These problems all can make the polyimide fiber after imidizate process and paper properties thereof be greatly affected.
Summary of the invention
In order to overcome the defect that above-mentioned prior art exists, the object of the present invention is to provide a kind of polyimide fiber paper adding potassium titanate crystal whisker and preparation method thereof, the present invention utilizes the potassium titanate crystal whisker of silane coupler modified process by adding, improve the strength character of polyimide fiber paper; Produce fiber hybrid effect by polyimide fiber, potassium titanate crystal whisker and PPTA-pulp/fibrid simultaneously, improve the combination property of polyimide fiber paper, better can be applied at high-temperature insulation material, filtering material, high temperature resistant radiation resistance material and cellular material.
For achieving the above object, the present invention adopts following technical scheme:
Add a polyimide fiber paper for potassium titanate crystal whisker, with weight parts, described polyimide fiber paper forms component and comprises: polyimide fiber: 45 ~ 60 parts; Para-aramid fiber: 32 ~ 49 parts; Modification potassium titanate crystal whisker: 6 ~ 12 parts.
Further, described para-aramid fiber is one or more in PPTA-pulp fiber or p-aramid fiber fibrid.
Further, described polyimide fiber length 4 ~ 7mm, fiber number 1.0 ~ 2.0D, initial pyrolyzation temperature is 560 DEG C; Modification potassium titanate crystal whisker utilizes silane coupler to carry out potassium titanate crystal whisker, and modification obtains.
Further, described potassium titanate crystal whisker is potassium hexatitanate, and performance is as follows: the pH of its aqueous dispersion liquid is 7 ~ 9, and diameter of whiskers is 0.8 ~ 1.5 μm, and whisker length is 30 ~ 100 μm, and whisker length-width ratio is 20 ~ 125, and whisker fusing point is 1300 ~ 1370 DEG C.
Add a preparation method for the polyimide fiber paper of potassium titanate crystal whisker, comprise the following steps:
Step 1: utilized by polyimide fiber ultrasonic disperse process to obtain pulp suspension (A);
Step 2: one or more fibers in p-aramid fiber fibrid, PPTA-pulp fiber are discongested the obtained pulp suspension (B) of dispersion through fibrillation process;
Step 3: utilize silane coupler to carry out modification to potassium titanate crystal whisker and obtain modification potassium titanate crystal whisker, drying for standby;
Step 4: mixed by modification potassium titanate crystal whisker obtained with step 3 for pulp suspension (B) obtained for step 2, discongests the obtained pulp suspension (C) of dispersion;
Step 5: discongest after pulp suspension (A) obtained for step 1 is mixed with the pulp suspension (C) obtained through step 4 and disperse obtained pulp suspension (D);
Step 6: shaping of being manufactured paper with pulp on oblique net paper machine by the pulp suspension (D) that step 5 is obtained, also carrying out hot pressing further on hot press obtains polyimide fiber paper for squeezing, drying.
Further, in step 1, polyimide fiber ultrasonic disperse treatment conditions are: ultrasonic power: 360 ~ 700W, sonication treatment time: 15 ~ 100min, mass concentration during process: 0.25% ~ 2.5%.
Further, in step 3, silane coupler is KH-570, and silane coupler consumption is 0.5 ~ 3.5% of potassium titanate crystal whisker quality.
Further, in the mixture that in step 4, modification potassium titanate crystal whisker and pulp suspension (B) are mixed to get, the mass concentration of modification potassium titanate crystal whisker is 0.5 ~ 8%.
Further, the pulp suspension (D) in step 5 comprises the modification potassium titanate crystal whisker of the polyimide fiber of 45 ~ 60 weight portions, the para-aramid fiber of 32 ~ 49 weight portions and 6 ~ 12 weight portions.
Further, a kind of preparation method adding the polyimide fiber paper of potassium titanate crystal whisker, comprises the following steps:
Step 1: utilized by polyimide fiber ultrasonic disperse process to obtain pulp suspension (A), ultrasonic treatment conditions: ultrasonic power: 600W, sonication treatment time: 35min, the mass concentration of bone dry fiber during process: 0.5%.
Step 2: p-aramid fiber fibrid is discongested the obtained pulp suspension (B) of dispersion through fibrillation process;
Step 3: utilize KH-570 silane coupler to carry out modification to potassium titanate crystal whisker, silane coupler consumption is 3% of potassium titanate crystal whisker quality, obtains modification potassium titanate crystal whisker, drying for standby;
Step 4: modification potassium titanate crystal whisker obtained with step 3 for pulp suspension (B) obtained for step 2 is mixed to get mixture, and wherein the mass concentration of potassium titanate crystal whisker is 2%, then discongest the obtained pulp suspension (C) of dispersion;
Step 5: pulp suspension (A) obtained for step 1 is mixed with the pulp suspension (C) obtained through step 4, controlling polyimide fiber component is 50 weight portions, para-aramid fiber component is 40 weight portions, modification potassium titanate crystal whisker component is 10 weight portions, discongests the obtained pulp suspension (D) of dispersion;
Step 6: shaping of being manufactured paper with pulp on oblique net paper machine by the pulp suspension (D) that step 5 is obtained, also carrying out hot pressing further on hot press obtains polyimide fiber paper for squeezing, drying.
Compared with prior art, Advantageous Effects of the present invention is:
The character of polyimide fiber is very stable, surface passivation, and polyimide fiber is due to higher strength modulus and the higher rigidity of strand, even if seminar's early-stage Study finds also can not produce fibrillation phenomenon through overground making beating process, therefore polyimide fiber is caused very easily to wad a quilt with cotton poly-, difficult dispersion.The present invention disperses polyimide fiber by ultrasonic wave, and the cavitation effect produced by ultrasonic process acts on fibre morphology and ultra microstructure, improves its dispersion effect in water, and then improves paper-forming evenness.
Another Advantageous Effects of the present invention is:
Potassium titanate crystal whisker has excellent mechanical property, stable chemical property, excellent corrosion resistance, heat-resisting thermal insulation, ABRASION RESISTANCE, high electric insulating quality, and its intensity far exceeds conventional glass fibre, carbon fiber, Kafra fiber etc.Adding utilizes silane coupler to carry out modification to potassium titanate crystal whisker, silane coupler hydrolysis generates the oligosiloxane compound with linear structure, complicated parcel is formed on potassium titanate crystal whisker surface, whisker and specific area large, whisker surface is defined between PPTA-pulp/fibrid that surface-activity is high, silane coupler, the coefficient boundary layer of fiber, form " fiber-whisker " small cladding, thus make whisker, polyimide fiber, higher interface cohesion is produced between PPTA-pulp/fibrid, improve the combination property of polyimide fiber paper.
Another Advantageous Effects of the present invention is:
PPTA-pulp fiber surface is lint shape, filoplume is abundant, fiber axis caudad fibril change into tip-like, p-aramid fiber fibrid is nonrigid film-form pleated structure, form fine (length 0.4 ~ 1.2mm), this makes Fanglun slurry cake/fibrid specific area large (8 ~ 12m2/g), surface-activity is high, thus making itself and long fiber, aqueous medium and interlaminar resin more easily form hydrogen bond, general performance is dispersiveness good in aqueous medium, excellent sheet forming quality and composite effect better with resin.Make full use of the excellent specific property of PPTA-pulp/fibrid as viscose fibre, improve the interface bond strength of polyimide fiber paper, produce fiber hybrid effect by polyimide fiber, potassium titanate crystal whisker and PPTA-pulp/fibrid simultaneously, improve the combination property of polyimide fiber paper, better can be applied at high-temperature insulation material, filtering material, high temperature resistant radiation resistance material and cellular material.
Accompanying drawing explanation
Fig. 1 is process flow diagram of the present invention;
Fig. 2 is potassium titanate crystal whisker and produce " fiber-whisker " small cladding structure SEM to ppta-pulp fibre surface and scheme (a: × 15000; B: × 50000);
Fig. 3 is potassium titanate crystal whisker and produce " fiber-whisker " small cladding structure SEM to aramid fiber fibrid surface and scheme (× 50000).
Detailed description of the invention
Below in conjunction with accompanying drawing, embodiments of the present invention are described in further detail:
See Fig. 1, a kind of preparation method adding the polyimide fiber paper of potassium titanate crystal whisker, comprises the following steps:
Step 1: utilized by polyimide fiber ultrasonic disperse process to obtain pulp suspension (A), ultrasonic treatment conditions: ultrasonic power: 360 ~ 700W, sonication treatment time: 15 ~ 100min, the mass concentration of bone dry fiber during process: 0.25% ~ 2.5%.
Step 2: one or more fibers in p-aramid fiber fibrid, PPTA-pulp fiber are discongested the obtained pulp suspension (B) of dispersion through fibrillation process
Step 3: utilize KH-570 silane coupler to carry out modification to potassium titanate crystal whisker, silane coupler consumption is 0.5 ~ 3.5% of potassium titanate crystal whisker quality, obtains modification potassium titanate crystal whisker, drying for standby;
Step 4: modification potassium titanate crystal whisker obtained with step 3 for pulp suspension (B) obtained for step 2 is mixed to get mixture, wherein the mass concentration of modification potassium titanate crystal whisker is 0.5 ~ 8%, then discongests the obtained pulp suspension (C) of dispersion;
Step 5: pulp suspension (A) obtained for step 1 is mixed with the pulp suspension (C) obtained through step 4, controlling polyimide fiber component is 45 ~ 60 weight portions, para-aramid fiber component is 32 ~ 49 weight portions, modification potassium titanate crystal whisker component is 6 ~ 12 weight portions, discongests the obtained pulp suspension (D) of dispersion;
Step 6: shaping of being manufactured paper with pulp on oblique net paper machine by the pulp suspension (D) that step 5 is obtained, also carrying out hot pressing further on hot press obtains polyimide fiber paper for squeezing, drying.
Below in conjunction with embodiment, the present invention is described in further detail:
Embodiment 1
Step 1: utilized by polyimide fiber ultrasonic disperse process to obtain pulp suspension (A), ultrasonic treatment conditions: ultrasonic power: 400W, sonication treatment time: 40min, the mass concentration of bone dry fiber during process: 1.2%;
Step 2: p-aramid fiber fibrid is discongested the obtained pulp suspension (B) of dispersion through fibrillation process;
Step 3: utilize KH-570 silane coupler to carry out modification to potassium titanate crystal whisker, silane coupler consumption is 3% of potassium titanate crystal whisker quality, obtains modification potassium titanate crystal whisker, drying for standby;
Step 4: modification potassium titanate crystal whisker obtained with step 3 for pulp suspension (B) obtained for step 2 is mixed to get mixture, and wherein the mass concentration of potassium titanate crystal whisker is 5%, then discongest the obtained pulp suspension (C) of dispersion;
Step 5: pulp suspension (A) obtained for step 1 is mixed with the pulp suspension (C) obtained through step 4, controlling polyimide fiber component is 60 weight portions, para-aramid fiber component is 35 weight portions, modification potassium titanate crystal whisker component is 7 weight portions, discongests the obtained pulp suspension (D) of dispersion;
Step 6: shaping of being manufactured paper with pulp on oblique net paper machine by the pulp suspension (D) that step 5 is obtained, also carrying out hot pressing further on hot press obtains polyimide fiber paper for squeezing, drying.
Embodiment 2
Step 1: utilized by polyimide fiber ultrasonic disperse process to obtain pulp suspension (A), ultrasonic treatment conditions: ultrasonic power: 650W, sonication treatment time: 70min, the mass concentration of bone dry fiber during process: 0.25%;
Step 2: p-aramid fiber fibrid is discongested the obtained pulp suspension (B) of dispersion through fibrillation process;
Step 3: utilize KH-570 silane coupler to carry out modification to potassium titanate crystal whisker, silane coupler consumption is 3.5% of potassium titanate crystal whisker quality, obtains modification potassium titanate crystal whisker, drying for standby;
Step 4: modification potassium titanate crystal whisker obtained with step 3 for pulp suspension (B) obtained for step 2 is mixed to get mixture, and wherein the mass concentration of potassium titanate crystal whisker is 5%, then discongest the obtained pulp suspension (C) of dispersion;
Step 5: pulp suspension (A) obtained for step 1 is mixed with the pulp suspension (C) obtained through step 4, controlling polyimide fiber component is 50 weight portions, para-aramid fiber component is 38 weight portions, modification potassium titanate crystal whisker component is 12 weight portions, discongests the obtained pulp suspension (D) of dispersion;
Step 6: shaping of being manufactured paper with pulp on oblique net paper machine by the pulp suspension (D) that step 5 is obtained, also carrying out hot pressing further on hot press obtains polyimide fiber paper for squeezing, drying.
Embodiment 3
Step 1: utilized by polyimide fiber ultrasonic disperse process to obtain pulp suspension (A), ultrasonic treatment conditions: ultrasonic power: 600W, sonication treatment time: 35min, the mass concentration of bone dry fiber during process: 0.5%.
Step 2: p-aramid fiber fibrid is discongested the obtained pulp suspension (B) of dispersion through fibrillation process;
Step 3: utilize KH-570 silane coupler to carry out modification to potassium titanate crystal whisker, silane coupler consumption is 3% of potassium titanate crystal whisker quality, obtains modification potassium titanate crystal whisker, drying for standby;
Step 4: modification potassium titanate crystal whisker obtained with step 3 for pulp suspension (B) obtained for step 2 is mixed to get mixture, and wherein the mass concentration of potassium titanate crystal whisker is 2%, then discongest the obtained pulp suspension (C) of dispersion;
Step 5: pulp suspension (A) obtained for step 1 is mixed with the pulp suspension (C) obtained through step 4, controlling polyimide fiber component is 50 weight portions, para-aramid fiber component is 40 weight portions, modification potassium titanate crystal whisker component is 10 weight portions, discongests the obtained pulp suspension (D) of dispersion;
Step 6: shaping of being manufactured paper with pulp on oblique net paper machine by the pulp suspension (D) that step 4 is obtained, also carrying out hot pressing further on hot press obtains polyimide fiber paper for squeezing, drying.
Embodiment 4
Step 1: utilized by polyimide fiber ultrasonic disperse process to obtain pulp suspension (A), ultrasonic treatment conditions: ultrasonic power: 500W, sonication treatment time: 25min, the mass concentration of bone dry fiber during process: 1.0%;
Step 2: PPTA-pulp fiber is discongested the obtained pulp suspension (B) of dispersion through fibrillation process;
Step 3: utilize KH-570 silane coupler to carry out modification to potassium titanate crystal whisker, silane coupler consumption is 2.5% of potassium titanate crystal whisker quality, obtains modification potassium titanate crystal whisker, drying for standby;
Step 4: modification potassium titanate crystal whisker obtained with step 3 for pulp suspension (B) obtained for step 2 is mixed to get mixture, and wherein the mass concentration of potassium titanate crystal whisker is 7.5%, then discongest the obtained pulp suspension (C) of dispersion;
Step 5: pulp suspension (A) obtained for step 1 is mixed with the pulp suspension (C) obtained through step 4, controlling polyimide fiber component is 58 weight portions, para-aramid fiber component is 35 weight portions, modification potassium titanate crystal whisker component is 7 weight portions, discongests the obtained pulp suspension (D) of dispersion;
Step 6: shaping of being manufactured paper with pulp on oblique net paper machine by the pulp suspension (D) that step 5 is obtained, also carrying out hot pressing further on hot press obtains polyimide fiber paper for squeezing, drying.
Embodiment 5
Step 1: utilized by polyimide fiber ultrasonic disperse process to obtain pulp suspension (A), ultrasonic treatment conditions: ultrasonic power: 650W, sonication treatment time: 55min, the mass concentration of bone dry fiber during process: 2.0%;
Step 2: PPTA-pulp fiber and external aramid fiber fibrid blended fiber are discongested disperse obtained pulp suspension (B) through fibrillation process;
Step 3: utilize KH-570 silane coupler to carry out modification to potassium titanate crystal whisker, silane coupler consumption is 2.5% of potassium titanate crystal whisker quality, obtains modification potassium titanate crystal whisker, drying for standby;
Step 4: modification potassium titanate crystal whisker obtained with step 3 for pulp suspension (B) obtained for step 2 is mixed to get mixture, and wherein the mass concentration of potassium titanate crystal whisker is 3.5%, then discongest the obtained pulp suspension (C) of dispersion;
Step 5: pulp suspension (A) obtained for step 1 is mixed with the pulp suspension (C) obtained through step 4, controlling polyimide fiber component is 58 weight portions, para-aramid fiber component is 35 weight portions, modification potassium titanate crystal whisker component is 7 weight portions, discongests the obtained pulp suspension (D) of dispersion;
Step 6: shaping of being manufactured paper with pulp on oblique net paper machine by the pulp suspension (D) that step 5 is obtained, also carrying out hot pressing further on hot press obtains polyimide fiber paper for squeezing, drying.
Embodiment 6
Step 1: utilized by polyimide fiber ultrasonic disperse process to obtain pulp suspension (A), ultrasonic treatment conditions: ultrasonic power: 550W, sonication treatment time: 80min, the mass concentration of bone dry fiber during process: 2.5%;
Step 2: PPTA-pulp fiber and external aramid fiber fibrid blended fiber are discongested disperse obtained pulp suspension (B) through fibrillation process;
Step 3: utilize KH-570 silane coupler to carry out modification to potassium titanate crystal whisker, silane coupler consumption is 3% of potassium titanate crystal whisker quality, obtains modification potassium titanate crystal whisker, drying for standby;
Step 4: modification potassium titanate crystal whisker obtained with step 3 for pulp suspension (B) obtained for step 2 is mixed to get mixture, and wherein the mass concentration of potassium titanate crystal whisker is 6%, then discongest the obtained pulp suspension (C) of dispersion;
Step 5: pulp suspension (A) obtained for step 1 is mixed with the pulp suspension (C) obtained through step 4, controlling polyimide fiber component is 60 weight portions, para-aramid fiber component is 32 weight portions, modification potassium titanate crystal whisker component is 8 weight portions, discongests the obtained pulp suspension (D) of dispersion;
Step 6: shaping of being manufactured paper with pulp on oblique net paper machine by the pulp suspension (D) that step 5 is obtained, also carrying out hot pressing further on hot press obtains polyimide fiber paper for squeezing, drying.
Embodiment 7
Step 1: utilized by polyimide fiber ultrasonic disperse process to obtain pulp suspension (A), ultrasonic treatment conditions: ultrasonic power: 360W, sonication treatment time: 100min, the mass concentration of bone dry fiber during process: 2.5%;
Step 2: PPTA-pulp fiber and external aramid fiber fibrid blended fiber are discongested disperse obtained pulp suspension (B) through fibrillation process;
Step 3: utilize KH-570 silane coupler to carry out modification to potassium titanate crystal whisker, silane coupler consumption is 0.5% of potassium titanate crystal whisker quality, obtains modification potassium titanate crystal whisker, drying for standby;
Step 4: modification potassium titanate crystal whisker obtained with step 3 for pulp suspension (B) obtained for step 2 is mixed to get mixture, and wherein the mass concentration of potassium titanate crystal whisker is 0.5%, then discongest the obtained pulp suspension (C) of dispersion;
Step 5: pulp suspension (A) obtained for step 1 is mixed with the pulp suspension (C) obtained through step 4, controlling polyimide fiber component is 45 weight portions, para-aramid fiber component is 32 weight portions, modification potassium titanate crystal whisker component is 6 weight portions, discongests the obtained pulp suspension (D) of dispersion;
Step 6: shaping of being manufactured paper with pulp on oblique net paper machine by the pulp suspension (D) that step 5 is obtained, also carrying out hot pressing further on hot press obtains polyimide fiber paper for squeezing, drying.
Embodiment 8
Step 1: utilized by polyimide fiber ultrasonic disperse process to obtain pulp suspension (A), ultrasonic treatment conditions: ultrasonic power: 700W, sonication treatment time: 15min, the mass concentration of bone dry fiber during process: 0.25%;
Step 2: PPTA-pulp fiber and external aramid fiber fibrid blended fiber are discongested disperse obtained pulp suspension (B) through fibrillation process;
Step 3: utilize KH-570 silane coupler to carry out modification to potassium titanate crystal whisker, silane coupler consumption is 3.5% of potassium titanate crystal whisker quality, obtains modification potassium titanate crystal whisker, drying for standby;
Step 4: modification potassium titanate crystal whisker obtained with step 3 for pulp suspension (B) obtained for step 2 is mixed to get mixture, and wherein the mass concentration of potassium titanate crystal whisker is 10%, then discongest the obtained pulp suspension (C) of dispersion;
Step 5: pulp suspension (A) obtained for step 1 is mixed with the pulp suspension (C) obtained through step 4, controlling polyimide fiber component is 60 weight portions, para-aramid fiber component is 49 weight portions, modification potassium titanate crystal whisker component is 12 weight portions, discongests the obtained pulp suspension (D) of dispersion;
Step 6: shaping of being manufactured paper with pulp on oblique net paper machine by the pulp suspension (D) that step 5 is obtained, also carrying out hot pressing further on hot press obtains polyimide fiber paper for squeezing, drying.
Claims (10)
1. add a polyimide fiber paper for potassium titanate crystal whisker, it is characterized in that, with weight parts, described polyimide fiber paper forms component and comprises: polyimide fiber: 45 ~ 60 parts; Para-aramid fiber: 32 ~ 49 parts; Modification potassium titanate crystal whisker: 6 ~ 12 parts.
2. described a kind of polyimide fiber paper adding potassium titanate crystal whisker according to claim 1, is characterized in that, described para-aramid fiber is one or more in PPTA-pulp fiber or p-aramid fiber fibrid.
3. described a kind of polyimide fiber paper adding potassium titanate crystal whisker according to claim 1, it is characterized in that, described polyimide fiber length 4 ~ 7mm, fiber number 1.0 ~ 2.0D, initial pyrolyzation temperature is 560 DEG C; Modification potassium titanate crystal whisker utilizes silane coupler to carry out potassium titanate crystal whisker, and modification obtains.
4. described a kind of polyimide fiber paper adding potassium titanate crystal whisker according to claim 1, it is characterized in that, described potassium titanate crystal whisker is potassium hexatitanate, performance is as follows: the pH of its aqueous dispersion liquid is 7 ~ 9, diameter of whiskers is 0.8 ~ 1.5 μm, whisker length is 30 ~ 100 μm, and whisker length-width ratio is 20 ~ 125, and whisker fusing point is 1300 ~ 1370 DEG C.
5. add a preparation method for the polyimide fiber paper of potassium titanate crystal whisker, it is characterized in that, comprise the following steps:
Step 1: utilized by polyimide fiber ultrasonic disperse process to obtain pulp suspension (A);
Step 2: one or more fibers in p-aramid fiber fibrid, PPTA-pulp fiber are discongested the obtained pulp suspension (B) of dispersion through fibrillation process;
Step 3: utilize silane coupler to carry out modification to potassium titanate crystal whisker and obtain modification potassium titanate crystal whisker, drying for standby;
Step 4: mixed by modification potassium titanate crystal whisker obtained with step 3 for pulp suspension (B) obtained for step 2, discongests the obtained pulp suspension (C) of dispersion;
Step 5: discongest after pulp suspension (A) obtained for step 1 is mixed with the pulp suspension (C) obtained through step 4 and disperse obtained pulp suspension (D);
Step 6: shaping of being manufactured paper with pulp on oblique net paper machine by the pulp suspension (D) that step 5 is obtained, also carrying out hot pressing further on hot press obtains polyimide fiber paper for squeezing, drying.
6. a kind of preparation method adding the polyimide fiber paper of potassium titanate crystal whisker according to claim 5, it is characterized in that, in step 1, polyimide fiber ultrasonic disperse treatment conditions are: ultrasonic power: 360 ~ 700W, sonication treatment time: 15 ~ 100min, mass concentration during process: 0.25% ~ 2.5%.
7. a kind of preparation method adding the polyimide fiber paper of potassium titanate crystal whisker according to claim 5, is characterized in that, in step 3, silane coupler is KH-570, and silane coupler consumption is 0.5 ~ 3.5% of potassium titanate crystal whisker quality.
8. a kind of preparation method adding the polyimide fiber paper of potassium titanate crystal whisker according to claim 5, it is characterized in that, in the mixture that in step 4, modification potassium titanate crystal whisker and pulp suspension (B) are mixed to get, the mass concentration of modification potassium titanate crystal whisker is 0.5 ~ 8%.
9. a kind of preparation method adding the polyimide fiber paper of potassium titanate crystal whisker according to claim 5, it is characterized in that, the pulp suspension (D) in step 5 comprises the modification potassium titanate crystal whisker of the polyimide fiber of 45 ~ 60 weight portions, the para-aramid fiber of 32 ~ 49 weight portions and 6 ~ 12 weight portions.
10. a kind of preparation method adding the polyimide fiber paper of potassium titanate crystal whisker according to claim 5, is characterized in that, comprise the following steps:
Step 1: utilized by polyimide fiber ultrasonic disperse process to obtain pulp suspension (A), ultrasonic treatment conditions: ultrasonic power: 600W, sonication treatment time: 35min, the mass concentration of bone dry fiber during process: 0.5%;
Step 2: p-aramid fiber fibrid is discongested the obtained pulp suspension (B) of dispersion through fibrillation process;
Step 3: utilize KH-570 silane coupler to carry out modification to potassium titanate crystal whisker, silane coupler consumption is 3% of potassium titanate crystal whisker quality, obtains modification potassium titanate crystal whisker, drying for standby;
Step 4: modification potassium titanate crystal whisker obtained with step 3 for pulp suspension (B) obtained for step 2 is mixed to get mixture, and wherein the mass concentration of potassium titanate crystal whisker is 2%, then discongest the obtained pulp suspension (C) of dispersion;
Step 5: pulp suspension (A) obtained for step 1 is mixed with the pulp suspension (C) obtained through step 4, controlling polyimide fiber component is 50 weight portions, para-aramid fiber component is 40 weight portions, modification potassium titanate crystal whisker component is 10 weight portions, discongests the obtained pulp suspension (D) of dispersion;
Step 6: shaping of being manufactured paper with pulp on oblique net paper machine by the pulp suspension (D) that step 5 is obtained, also carrying out hot pressing further on hot press obtains polyimide fiber paper for squeezing, drying.
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