CN103806342A - Polyimide paper honeycomb core and preparation method thereof - Google Patents
Polyimide paper honeycomb core and preparation method thereof Download PDFInfo
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- CN103806342A CN103806342A CN201410051144.XA CN201410051144A CN103806342A CN 103806342 A CN103806342 A CN 103806342A CN 201410051144 A CN201410051144 A CN 201410051144A CN 103806342 A CN103806342 A CN 103806342A
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Abstract
The invention discloses a polyimide paper honeycomb core and a preparation method thereof. The polyimide paper honeycomb core is prepared by the following methods: (1) performing gluing treatment, namely coating a polyimide adhesive on the surface of polyimide paper, superposing multilayer glued polyimide paper in a staggered mode, and finally performing hot-pressing to prepare a honeycomb laminate by utilizing a hot press; (2) performing setting treatment, namely stretching the honeycomb laminate, forming regular hexagon honeycomb hole lattices, and setting in a drying box to preparw white honeycomb blocks; (3) performing impregnation treatment, namely impregnating and curing the white honeycomb blocks to prepare the polyimide paper honeycomb core. The polyimide paper honeycomb core prepared by the method has the characteristics of high temperature resistance and low moisture absorption property, and the strength of the polyimide paper honeycomb core can be further improved.
Description
Technical field
The present invention relates to a kind of polyimides paper honeycomb core and preparation method thereof, belong to paper technology and insulating materials and manufacture field.
Background technology
Honeycomb core is made according to nature honeycomb structure principle, and it is to adopt high-strength core by techniques such as bonding, stretchings, connects into the orthohexagonal structure of numerous hollow solid, forms an overall stressed member.Conventional comb core has aluminium honeycomb core and paper honeycomb core.The price of aluminium honeycomb core is lower, serviceability temperature is higher, but because the density of aluminium is higher, can not serve as electromagnetic wave transparent material, is mainly used in the insensitive building field of weight.And paper honeycomb core is prepared from aramid paper conventionally, but the maximum operation (service) temperature of aramid paper can not exceed 200 ℃.In addition, because aramid fiber itself contains amide group, polarity is strong, and easily water suction, through impregnation, is solidified and made after aramid paper honeycomb, and exposed aramid paper still has extremely strong water imbibition.In extreme weather, can decrease the service life of aramid paper honeycomb core like this.
Polyimide fiber is the highest synthetic fiber of current serviceability temperature, can at 250 ℃-300 ℃, use for a long time.Polyimide fiber has high strength and modulus, and its maximum intensity can reach 5.8-6.3GPa, and modulus can reach 280-340GPa.Its mechanical property is considerably beyond aramid fiber.Therefore, polyimide fiber will be far superior to aramid fiber compared with aramid fiber in intensity.Meanwhile, polyimide fiber is all more superior at aspects such as light resistance, heat resistance, water imbibitions.
In view of the superior function of polyimide fiber, polyimide fiber has been applied to field of papermaking by we, and the polyimides paper that my company produces has not only overcome the shortcomings such as aramid paper heatproof is low, easy moisture absorption, and has the high feature such as light resistance, anti-flammability.
Summary of the invention
Have for overcoming the paper honeycomb core of prior art that serviceability temperature is low, the defect of poor water resistance, the object of the present invention is to provide a kind of polyimides paper honeycomb core, there is feature high temperature resistant, that hygroscopicity is little and intensity is high.
Another object of the present invention is to provide a kind of preparation method of polyimides paper honeycomb core, the polyimides paper honeycomb core that adopts the method to prepare has the feature high temperature resistant, hygroscopicity is little, can also further improve the intensity of polyimides paper honeycomb core simultaneously.
The technical solution adopted in the present invention is as follows for achieving the above object:
A kind of polyimides paper honeycomb core, is characterized in that, carries out successively gluing, sizing and impregnation three step treatment process prepare by polyimides paper.
A preparation method for polyimides paper honeycomb core, is characterized in that, is prepared from by the following method:
1) gluing processing: coat polyimides glue on the surface of polyimides paper, then, by superimposed the polyimides paper staggered floor after multilayer gluing, finally utilize hot press hot pressing, make the folded piece of honeycomb;
2) heat treatment: folded honeycomb piece is stretched, form regular hexagon honeycomb hole lattice; In baking oven, shape afterwards, make white honeycomb block;
3) dipping process: by white honeycomb block carry out impregnation solidify after, make polyimides paper honeycomb core.
As the preferred scheme of one of the present invention, in step 1), described polyimides paper is to be prepared from through manufacturing paper with pulp take polyimide fiber as main raw material.
As the preferred scheme of one of the present invention, in step 1), polyimides glue is to be polymerized by dianhydride and diamines, and the viscosity of described polyimides glue is 10s/50ml-60s/50ml.
As the preferred scheme of one of the present invention, in step 1), when hot pressing, first preheating 40-50min at 70-90 ℃, then gel 90-120min at 120-140 ℃ finally solidifies 3-5h at 160-250 ℃, and hot pressing pressure is 5-7MPa.By preferably rational technological parameter, can guarantee the intensity of node herein, affect intensity otherwise degraded occurs polyimides glue.
As the preferred scheme of one of the present invention, in step 2) in, in heat treatment process, controlling temperature is 100 ℃-400 ℃, the time is 10min-60min.
As the preferred scheme of one of the present invention, in step 3) in, described dipping solution comprises polyimide resin and organic solvent; Wherein, the quality of described polyimide resin is the 5-50% of dipping solution gross mass, and polyimide resin is to be polymerized by dianhydride and diamines.
Described dianhydride is the one in equal benzene dianhydride (PMDA), biphenyl dianhydride (BPDA), benzophenone dianhydride (BTDA), diphenyl ether dianhydride (ODPA), diphenyl sulfide dianhydride (TDPA), diphenyl sulfone dianhydride (SDPA), triphen two ether dianhydrides (HQDPA), Bisphenol A Type Diether Dianhydride (BPADA), Bisphenol F type two ether dianhydrides (BPFDA) and '-biphenyl diphenol two ether dianhydrides.
Described diamines is p-phenylenediamine (PPD) (PPD), m-phenylene diamine (MPD) (MPD), diphenylmethane diamine (MDA), diphenyl ether diamines (ODA), triphen two ether diamines (HQDPA), 4, 4 '-bis-(4-amino-benzene oxygen) biphenyl (BAPB), 2, two [4-(4-amino-benzene oxygen) phenyl] propane (BAPP) of 2-, 5 (6)-amino-2-(4 '-aminophenyl) benzimidazoles (PABZ), 5-amino-2-(4-aminophenyl) benzoxazole (PABO), 2, one in 5-bis-(4-aminophenyl) pyrimidine (PRM).
As the preferred scheme of one of the present invention, in step 3) in, the impregnation time is 20min-60min, impregnation number of times is 3-10 time.
As the preferred scheme of one of the present invention, in step 3) in, after each impregnation, preheating 30-40min in 80 ℃ of baking ovens is then dried 90-100min at 130-140 ℃, and gel 2h at 200-250 ℃ finally solidifies 4-5h at 350 ℃.
Beneficial effect of the present invention is:
1, the present invention is directed to conventional paper honeycomb core, the features such as serviceability temperature is low, poor water resistance, propose a kind of brand-new polyimides paper honeycomb core and preparation method thereof.In the present invention, polyimides honeycomb fiberboard medium itself has the feature high temperature resistant, hygroscopicity is low, is used in conjunction with together with polyimide resin with polyimides glue, makes polyimides paper honeycomb have the performances such as high temperature resistant, hygroscopicity is low.
2, polyimides honeycomb core of the present invention, than traditional aluminium honeycomb core and aramid fiber honeycomb core, widen the application of honeycomb core in the high-end field such as space flight and aviation, submarine, expanded the application scale of polyimides, for the development of high-technology field provides certain support.
3, with respect to the production technology of traditional aramid paper honeycomb core, the present invention has adjusted the temperature of high-temperature shaping processing, overcome the restriction of traditional aramid paper honeycomb temperature resistant grade, further improved the intensity of polyimides paper honeycomb core, given full play to the advantage of polyimides paper honeycomb.
4, polyimide resin of the present invention have high strength, high-modulus, higher decomposition temperature, high-and low-temperature resistance, water absorption rate low, can certainly put out and the performance such as nontoxic.Polyimide resin is applied in the preparation of polyimides paper honeycomb core, has expanded the scope of application of polyimides paper honeycomb core.
Below in conjunction with concrete embodiment, the present invention is described in further detail.
The specific embodiment
Embodiment 1
The polyimides paper honeycomb core that the preparation space length of side is 1.83mm.Concrete steps are as follows:
(1) take thickness as the thick polyimides paper of 0.05mm is as raw material.The glue spreader that utilization speckles with core bar glue carries out gluing, then by superimposed the polyimides paper staggered floor after multilayer gluing, finally utilizes hot press hot pressing, makes the folded piece of honeycomb.Core bar glue is polyimides glue, is to be polymerized by equal benzene dianhydride and m-phenylene diamine (MPD), and viscosity is 30s/50ml.When hot pressing, first preheating 50min at 80 ℃, then 130 ℃ of gel 100min, last 250 ℃ of curing 4h, hot pressing pressure is 6MPa.
(2) after honeycomb block is stretched with the draw speed of 10mm/min with stretching-machine, form regular hexagon honeycomb hole lattice, 40min afterwards shapes under 300 ℃ of conditions in baking oven.Make white honeycomb block.
(3) white honeycomb block being carried out in cement dipping machine to impregnation solidifies;
Concrete, described dipping solution comprises polyimide resin and organic solvent; Wherein, the quality of described polyimide resin is 10% of dipping solution gross mass, and polyimide resin is to be polymerized by equal benzene dianhydride and p-phenylenediamine (PPD), and organic solvent is dimethylacetylamide.In present case, dialogue honeycomb block is carried out impregnation 5 times, and the impregnation time is 40min, and open assembly time is 30min.After each impregnation in 80 ℃ of baking ovens preheating 30min, then dry 100min, 200 ℃ of gel 2h, last 350 ℃ of curing 4h for 130 ℃.
(4) to impregnation solidify after honeycomb cut into slices, obtaining density is the polyimides paper honeycomb core of 75kg/m3.
After testing, 280 ℃ are processed 24h strength retention is 90%, 570 ℃ of the decomposition temperatures of polyimides paper honeycomb, and regain is 0.02%.
Embodiment 2
The polyimides paper honeycomb core that the preparation space length of side is 3.67mm.Concrete steps are as follows:
(1) take thickness as the thick polyimides paper of 0.08mm is as raw material.The glue spreader that utilization speckles with core bar glue carries out gluing, then by superimposed the polyimides paper staggered floor after multilayer gluing, finally utilizes hot press hot pressing, makes the folded piece of honeycomb.Core bar glue is polyimides glue, is to be polymerized by equal benzene dianhydride and m-phenylene diamine (MPD), and viscosity is 25s/50ml.When hot pressing, first preheating 40min at 90 ℃, then 120 ℃ of gel 120min, last 160 ℃ of curing 5h, hot pressing pressure is 5MPa.
(2) after honeycomb block is stretched with the draw speed of 5-20mm/min with stretching-machine, form regular hexagon honeycomb hole lattice, 60min afterwards shapes under 300 ℃ of conditions in baking oven.Make white honeycomb block.
(3) white honeycomb block being carried out in cement dipping machine to impregnation solidifies;
Concrete, dipping solution comprises polyimide resin and organic solvent; Wherein, the quality of described polyimide resin is 30% of dipping solution gross mass, and polyimide resin is to be polymerized by biphenyl dianhydride and m-phenylene diamine (MPD), and organic solvent is dimethyl formamide.In present case, dialogue honeycomb block is carried out impregnation 4 times, and the impregnation time is 60min, and open assembly time is 40min.After impregnation in 80 ℃ of baking ovens preheating 40min, 140 ℃ dry 90min, 230 ℃ of gel 1.5h, 350 ℃ of curing 5h.
(4) to impregnation solidify after honeycomb cut into slices, obtaining density is the polyimides paper honeycomb core of 68kg/m3.
After testing, 280 ℃ are processed 24h strength retention is 92%, 570 ℃ of the decomposition temperatures of polyimides paper honeycomb, and regain is 0.02%.
Embodiment 3
The polyimides paper honeycomb core that the preparation space length of side is 2.75mm.Concrete steps are as follows:
(1) take thickness as the thick polyimides paper of 0.13mm is as raw material.The glue spreader that utilization speckles with core bar glue carries out gluing, then by superimposed the polyimides paper staggered floor after multilayer gluing, finally utilizes hot press hot pressing, makes the folded piece of honeycomb.Core bar glue is polyimides glue, is to be polymerized by diphenyl ether dianhydride and m-phenylene diamine (MPD), and viscosity is 35s/50ml.When hot pressing, first preheating 50min at 70 ℃, then 140 ℃ of gel 90min, last 250 ℃ of curing 3h, hot pressing pressure is 7MPa.
(2) after honeycomb block is stretched with the draw speed of 10-15mm/min with stretching-machine, form regular hexagon honeycomb hole lattice, 80min afterwards shapes under 310 ℃ of conditions in baking oven.Make white honeycomb block.
(3) white honeycomb block being carried out in cement dipping machine to impregnation solidifies:
Concrete, dipping solution comprises polyimide resin and organic solvent; Wherein, the quality of described polyimide resin is 50% of dipping solution gross mass, and polyimide resin is to be polymerized by biphenyl dianhydride and diphenyl ether diamines, and organic solvent is dimethyl sulfoxide (DMSO).In present case, dialogue honeycomb block is carried out impregnation 3 times, and the impregnation time is 80min, and open assembly time is 40min.After impregnation in 80 ℃ of baking ovens preheating 40min, then 140 ℃ dry 90min, 250 ℃ of gel 1.5h afterwards, last 350 ℃ of curing 5h.
(4) to impregnation solidify after honeycomb cut into slices, obtaining density is the polyimides paper honeycomb core of 66kg/m3.
After testing, 280 ℃ are processed 24h strength retention is 91%, 570 ℃ of the decomposition temperatures of polyimides paper honeycomb, and regain is 0.02%.
It should be noted that, in preparation method of the present invention, polyimides paper is the paper take polyimide fiber as main raw material, is not singly to refer to the paper take polyimide fiber as raw material completely.Also comprise the polyimides paper that adds the fiber such as aramid fiber, carbon fiber.
Above-mentioned embodiment is only the preferred embodiment of the present invention; can not limit the scope of protection of the invention with this, the variation of any unsubstantiality that those skilled in the art does on basis of the present invention and replacement all belong to the present invention's scope required for protection.
Claims (10)
1. a polyimides paper honeycomb core, is characterized in that, carries out successively gluing, sizing and impregnation three step treatment process prepare by polyimides paper.
2. the preparation method of polyimides paper honeycomb core according to claim 1, is characterized in that, is prepared from by the following method:
1) gluing processing: coat polyimides glue on the surface of polyimides paper, then, by superimposed the polyimides paper staggered floor after multilayer gluing, finally utilize hot press hot pressing, make the folded piece of honeycomb;
2) heat treatment: folded honeycomb piece is stretched, form honeycomb hole lattice; In baking oven, shape afterwards, make white honeycomb block;
3) dipping process: by white honeycomb block carry out impregnation solidify after, make polyimides paper honeycomb core.
3. the preparation method of polyimides paper honeycomb core according to claim 2, is characterized in that: in step 1), described polyimides paper is to be prepared from through manufacturing paper with pulp take polyimide fiber as main raw material.
4. the preparation method of polyimides paper honeycomb core according to claim 2, is characterized in that: in step 1), described polyimides glue is to be polymerized by dianhydride and diamines, and the viscosity of described polyimides glue is 10s/50ml-60s/50ml.
5. the preparation method of polyimides paper honeycomb core according to claim 2, it is characterized in that: in step 1), when hot pressing, first preheating 40-50min at 70-90 ℃, then gel 90-120min at 120-140 ℃, finally at 160-250 ℃, solidify 3-5h, hot pressing pressure is 5-7MPa.
6. the preparation method of polyimides paper honeycomb core according to claim 2, is characterized in that: in step 2) in, in heat treatment process, controlling temperature is 100 ℃-400 ℃, the time is 10min-60min.
7. the preparation method of polyimides paper honeycomb core according to claim 2, is characterized in that: in step 3) in, described dipping solution comprises polyimide resin and organic solvent; Wherein, the quality of described polyimide resin is the 5-50% of dipping solution gross mass, and polyimide resin is to be polymerized by dianhydride and diamines.
8. the preparation method of polyimides paper honeycomb core according to claim 7, is characterized in that: described dianhydride is the one in equal benzene dianhydride, biphenyl dianhydride, benzophenone dianhydride, diphenyl ether dianhydride, diphenyl sulfide dianhydride, diphenyl sulfone dianhydride, triphen two ether dianhydrides, Bisphenol A Type Diether Dianhydride, Bisphenol F type two ether dianhydrides and '-biphenyl diphenol two ether dianhydrides; Described diamines is p-phenylenediamine (PPD), m-phenylene diamine (MPD), diphenylmethane diamine, diphenyl ether diamines, triphen two ether diamines, 4,4 '-bis-(4-amino-benzene oxygen) biphenyl, 2, two [4-(4-amino-benzene oxygen) phenyl] propane of 2-, 5 (6)-amino-2-(4 '-aminophenyl) benzimidazole, 5-amino-2-(4-aminophenyl) benzoxazole, 2, the one in 5-bis-(4-aminophenyl) pyrimidine.
9. the preparation method of polyimides paper honeycomb core according to claim 2, is characterized in that: in step 3) in, the impregnation time is 20min-60min, impregnation number of times is 3-10 time.
10. the preparation method of polyimides paper honeycomb core according to claim 9, it is characterized in that: in step 3) in, after each impregnation, preheating 30-40min in 80 ℃ of baking ovens, then at 130-140 ℃, dry 90-100min, gel 2h at 200-250 ℃ finally solidifies 4-5h at 350 ℃.
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Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN105369694A (en) * | 2015-09-29 | 2016-03-02 | 长春高琦聚酰亚胺材料有限公司 | Full-polyimide foam honeycomb and manufacturing method thereof |
| CN105666953A (en) * | 2016-03-10 | 2016-06-15 | 苏州芳磊蜂窝复合材料有限公司 | Aromatic polyoxadiazole fiber paper honeycomb |
| CN106147228A (en) * | 2016-07-05 | 2016-11-23 | 北京化工大学 | A kind of be wall material with polyimides sheet material cellular structural material and preparation method thereof |
| CN107379644A (en) * | 2017-07-26 | 2017-11-24 | 河北科技大学 | A kind of method for preparing carbon fiber comb core |
| CN109024953A (en) * | 2018-09-19 | 2018-12-18 | 广东星亿达科技有限公司 | Efficient soundproof plate |
| CN109677014A (en) * | 2018-12-19 | 2019-04-26 | 中航复合材料有限责任公司 | A kind of refractory honeycomb core material and preparation method thereof |
| CN109849479A (en) * | 2019-01-29 | 2019-06-07 | 连云港市工业投资集团有限公司 | A kind of honeycomb type carbon fibre composite trim panel and preparation method thereof |
| CN110091551A (en) * | 2018-01-31 | 2019-08-06 | 成都天府轨谷科技有限公司 | A kind of rail vehicle inner wall decorative composite material and preparation method thereof |
| CN111421898A (en) * | 2020-04-01 | 2020-07-17 | 南京南大波平电子信息有限公司 | Preparation method of light flexible high-temperature-resistant honeycomb core material |
| CN112223772A (en) * | 2020-08-31 | 2021-01-15 | 北京卫星制造厂有限公司 | Preparation method of polyimide film honeycomb |
| CN114228258A (en) * | 2021-12-17 | 2022-03-25 | 芜湖创联新材料科技有限公司 | Paper honeycomb capable of improving node strength and gum dipping appearance and preparation method thereof |
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Cited By (13)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105369694A (en) * | 2015-09-29 | 2016-03-02 | 长春高琦聚酰亚胺材料有限公司 | Full-polyimide foam honeycomb and manufacturing method thereof |
| CN105666953A (en) * | 2016-03-10 | 2016-06-15 | 苏州芳磊蜂窝复合材料有限公司 | Aromatic polyoxadiazole fiber paper honeycomb |
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| CN107379644A (en) * | 2017-07-26 | 2017-11-24 | 河北科技大学 | A kind of method for preparing carbon fiber comb core |
| CN110091551A (en) * | 2018-01-31 | 2019-08-06 | 成都天府轨谷科技有限公司 | A kind of rail vehicle inner wall decorative composite material and preparation method thereof |
| CN110091551B (en) * | 2018-01-31 | 2021-08-24 | 成都天府轨谷科技有限公司 | Composite material for decorating inner wall of rail transit vehicle and preparation method thereof |
| CN109024953A (en) * | 2018-09-19 | 2018-12-18 | 广东星亿达科技有限公司 | Efficient soundproof plate |
| CN109677014A (en) * | 2018-12-19 | 2019-04-26 | 中航复合材料有限责任公司 | A kind of refractory honeycomb core material and preparation method thereof |
| CN109849479A (en) * | 2019-01-29 | 2019-06-07 | 连云港市工业投资集团有限公司 | A kind of honeycomb type carbon fibre composite trim panel and preparation method thereof |
| CN111421898A (en) * | 2020-04-01 | 2020-07-17 | 南京南大波平电子信息有限公司 | Preparation method of light flexible high-temperature-resistant honeycomb core material |
| CN112223772A (en) * | 2020-08-31 | 2021-01-15 | 北京卫星制造厂有限公司 | Preparation method of polyimide film honeycomb |
| CN114228258A (en) * | 2021-12-17 | 2022-03-25 | 芜湖创联新材料科技有限公司 | Paper honeycomb capable of improving node strength and gum dipping appearance and preparation method thereof |
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Application publication date: 20140521 |
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