CN105220262A - A kind of polyimides (PI) pulp and preparation method thereof - Google Patents
A kind of polyimides (PI) pulp and preparation method thereof Download PDFInfo
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- CN105220262A CN105220262A CN201510532799.3A CN201510532799A CN105220262A CN 105220262 A CN105220262 A CN 105220262A CN 201510532799 A CN201510532799 A CN 201510532799A CN 105220262 A CN105220262 A CN 105220262A
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Abstract
The present invention relates to the preparation method of a kind of polyimides (PI) pulp, comprise the following steps: the polyimide fiber that is prepared into will be synthesized by aromatic dianhydride and aromatic diamine to cut into through cutting mechanics the short fiber of 2-30mm, and then be dispersed in water the suspension being made into 0.1%-20%; Suspension is discongested through disc mill, cut off, brooming 5-120min, makes the slurry of the abundant fibrillation of single fiber length 0.2-5mm; Slurry enters that concentration is 0.1-10mol/L, temperature is process 2-120 minute in the alkali lye of 5-80 DEG C after dehydration, after dehydrate after fully washing; Dried slurry is made loose polyimides pulp after fibrillation loosens process, and the specific area of pulp is 3-25m
2/ g.The preparation method of polyimides pulp provided by the invention, can prepare and have high-specific surface area, and surface is containing the polyimides pulp material enriching active function groups.
Description
Technical field:
The present invention relates to a kind of polyimides (PI) pulp and preparation method thereof, particularly synthesized by one or more aromatic dianhydride and one or more aromatic diamines and be prepared into polyimide fiber.
Background technology:
Polyimide material is the material of a class function admirable, possess high temperature resistant, low temperature resistant, radiation hardness, chemically-resistant solvent, the feature such as hydroscopicity is low, electrical insulation capability good, excellent in mechanical performance, good stability of the dimension, have wide application at high temperature resistant, low temperature resistant and other complicated chemical environmental areas and field of compound material.Polyimides is prepared into pulp material, not only possesses the performance of polyimides excellence, also have abundant filoplume structure, (specific area is 3-25m to add specific area
2/ g), surface, containing abundant active function groups, it can be used as interpolation material modified, add the contact area with matrix, enhance interfacial combined function, high-temperature insulation, adiabatic field can be applied to, the field of sealing technology of the media such as the soda acid of water, oil, hydro carbons and moderate strength.
Summary of the invention:
The object of the present invention is to provide a kind of method preparing polyimides pulp, its production process is simple, low production cost, can prepare and have excellent high temperature resistance, low temperature resistant, radiation hardness, chemically-resistant solvent, low hydroscopicity performance polyimides pulp.
A kind of preparation method of polyimides (PI) pulp, comprises the following steps:
A: the polyimide fiber that is prepared into will be synthesized by aromatic dianhydride and aromatic diamine to cut into through cutting mechanics the short fiber of 2-30mm, and then be dispersed in water the suspension being made into 0.1%-20%;
B: suspension is discongested through disc mill, cut off, brooming 5-120min, makes the slurry of the abundant fibrillation of single fiber length 0.2-5mm:
C: slurry enters that concentration is 0.1-10mol/L, temperature is process 2-120 minute in the alkali lye of 5-80 DEG C after dehydration, after dehydrate after fully washing;
D: dried slurry is made loose polyimides pulp after fibrillation loosens process, the specific area of pulp is 3-25m
2/ g.
The structural formula of the dianhydride adopted in steps A is aromatic dianhydride, includes but not limited to one or more in following structural:
The structural formula of the diamines adopted in steps A is aromatic diamines, includes but not limited to one or more in following structural:
The alkali lye adopted in step C is NaOH or the KOH aqueous solution, and the concentration of solution is 1-8mol/L.
In step C, the processing time of slurry in alkali lye is 20-80 minute, and the temperature of alkali lye is 20-60 DEG C.
Polyimides pulp preparation method provided by the invention, has production technology simple, the advantage of low production cost.
The present invention has following advantage:
1. adopt polyimides staple fibre to prepare polyimides pulp, be prepared by the defibrination technology of maturation, preparation efficiency is high, and technical process is controlled, and the process of enforcement is simple, with low cost.
2. the polyimides pulp material shape obtained is good, and fiber pulp average length, between 0.2-5mm, has very high specific area, is in 3-25m
2the interval of/g, adds the contact area with matrix, enhances interface performance.
3. the slurry of pair fiberizer output carries out base extraction, and treatment effeciency is high, and the polyimides pulp surface of acquisition has abundant active function groups, and add the binding ability with other matrixes, interface performance is excellent.
4. the polyimides pulp material prepared of the present invention, has excellent high and low temperature resistance, not brittle failure in-269 DEG C of liquid heliums, and place 120 hours at 300 DEG C, fibre strength conservation rate is 100%.
The polyimides pulp material of the preparation of said method has that reference area is large, pulp surface-active functional group enriches, high and low temperature resistance is good, the features such as dimensional performance is stable, high-temperature insulation, adiabatic field can be applied to, the field of sealing technology of the media such as the soda acid of water, oil, hydro carbons and moderate strength.
Below in conjunction with embodiment, the invention will be further described.
Detailed description of the invention:
Embodiment 1:
A: adopt dianhydride a-BPDA and diamines PPD synthesize and be prepared into polyimide fiber, cut into through cutting mechanics the staple fibre that length is 28mm, be then dispersed in water the suspension being made into 15%;
B: suspension is discongested through disc mill, cut off, brooming 100min, makes the slurry that average single fiber length is 0.5mm, fully fibrillation;
C: the NaOH alkaline solution treatment 70 minutes that through dehydration, slurry enters that concentration is 8mol/L, temperature is 40 DEG C, after dehydrate after fully washing.
D: dried slurry is made loose polyimides pulp after fibrillation loosens process, the specific area of pulp is 25m
2/ g.
According to polyimides pulp prepared by the method, the average length of described pulp fibers is 0.5mm, and specific area is 25m
2/ g.
Embodiment 2:
A: adopt dianhydride PMDA and diamines ODA and PPD synthesize and be prepared into polyimide fiber, cut into through cutting mechanics the staple fibre that length is 24mm, be then dispersed in water the suspension being made into 18%:
B: suspension is discongested through disc mill, cut off, brooming 80min, makes the slurry that average single fiber length is 1.3mm, fully fibrillation;
C: the NaOH alkaline solution treatment 80 minutes that through dehydration, slurry enters that concentration is 6mol/L, temperature is 30 DEG C, after dehydrate after fully washing.
D: dried slurry is made loose polyimides pulp after fibrillation loosens process, the specific area of pulp is 23m
2/ g.
According to polyimides pulp prepared by the method, the average length of described pulp fibers is 1.3mm, and specific area is 23m
2/ g.
Embodiment 3:
A: adopt dianhydride BTDA and ODPA and diamines DMB, DAP synthesize and are prepared into polyimide fiber, cut into through cutting mechanics the staple fibre that length is 15mm, be then dispersed in water the suspension being made into 10%;
B: suspension is discongested through disc mill, cut off, brooming 60min, makes the slurry that average single fiber length is 2.0mm, fully fibrillation;
C: the high temperature NaOH alkaline solution treatment 5 minutes that through dehydration, slurry enters that concentration is 5mol/L, temperature is 80 DEG C, after dehydrate after fully washing.
D: dried slurry is made loose polyimides pulp after fibrillation loosens process, the specific area of pulp is 10m
2/ g.
According to polyimides pulp prepared by the method, the average length of described pulp fibers is 2.0mm, and specific area is 10m
2/ g.
Embodiment 4:
A: adopt dianhydride BPDA and TDPA and diamines SDA and MPD synthesize and be prepared into polyimide fiber, cut into through cutting mechanics the staple fibre that length is 20mm, be then dispersed in water the suspension being made into 15%;
B: suspension is discongested through disc mill, cut off, brooming 120min, makes the slurry that average single fiber length is 1.0mm, fully fibrillation:
C: the NaOH alkaline solution treatment 120 minutes that through dehydration, slurry enters that concentration is 0.1mol/L, temperature is 5 DEG C, after dehydrate after fully washing.
D: dried slurry is made loose polyimides pulp after fibrillation loosens process, the specific area of pulp is 8m
2/ g.
According to polyimides pulp prepared by the method, the average length of described pulp fibers is 1.0mm, and specific area is 8m
2/ g.
Embodiment 5:
A: adopt dianhydride 6FDA and diamines ODA/TFDB/PPD synthesize and be prepared into polyimide fiber, cut into through cutting mechanics the staple fibre that length is 10mm, be then dispersed in water the suspension being made into 5%;
B: suspension is discongested through disc mill, cut off, brooming 30min, makes the slurry that average single fiber length is 4.9mm, fully fibrillation:
C: the NaOH alkaline solution treatment 20 minutes that through dehydration, slurry enters that concentration is 1mol/L, temperature is 20 DEG C, after dehydrate after fully washing.
D: dried slurry is made loose polyimides pulp after fibrillation loosens process, the specific area of pulp is 6m
2/ g.
According to polyimides pulp prepared by the method, the average length of described pulp fibers is 4.9mm, and specific area is 6m
2/ g.
Embodiment 6:
A: adopt dianhydride HQDPA and PMDA and diamines ODA and OTOL synthesize and be prepared into polyimide fiber, cut into through cutting mechanics the staple fibre that length is 5mm, be then dispersed in water the suspension being made into 17%;
B: suspension is discongested through disc mill, cut off, brooming 90min, makes the slurry that average single fiber length is 0.3mm, fully fibrillation;
C: the KOH alkaline solution treatment 75 minutes that through dehydration, slurry enters that concentration is 4mol/L, temperature is 35 DEG C, after dehydrate after fully washing.
D: dried slurry is made loose polyimides pulp after fibrillation loosens process, the specific area of pulp is 22m
2/ g.
According to polyimides pulp prepared by the method, the average length of described pulp fibers is 0.3mm, and specific area is 22m
2/ g.
Embodiment 7:
A: adopt dianhydride BPDA and PMDA and diamines PRM/ODA/AAQ synthesize and be prepared into polyimide fiber, cut into through cutting mechanics the staple fibre that length is 8mm, be then dispersed in water the suspension being made into 5%;
B: suspension is discongested through disc mill, cut off, brooming 100min, makes the slurry that average single fiber length is 0.8mm, fully fibrillation:
C: the KOH alkaline solution treatment 15 minutes that through dehydration, slurry enters that concentration is 7mol/L, temperature is 15 DEG C, after dehydrate after fully washing.
D: dried slurry is made loose polyimides pulp after fibrillation loosens process, the specific area of pulp is 19m
2/ g.
According to polyimides pulp prepared by the method, the average length of described pulp fibers is 0.8mm, and specific area is 19m
2/ g.
Embodiment 8:
A: adopt dianhydride BTDA/PMDA/TDPA and diamines PABZ/MPD/SDA synthesize and be prepared into polyimide fiber, cut into through cutting mechanics the staple fibre that length is 10mm, be then dispersed in water the suspension being made into 5%;
B: suspension is discongested through disc mill, cut off, brooming 110min, makes the slurry that average single fiber length is 1.0mm, fully fibrillation;
C: the high temperature NaOH alkaline solution treatment 30 minutes that through dehydration, slurry enters that concentration is 9mol/L, temperature is 75 DEG C, after dehydrate after fully washing.
D: dried slurry is made loose polyimides pulp after fibrillation loosens process, the specific area of pulp is 25m
2/ g.
According to polyimides pulp prepared by the method, the average length of described pulp fibers is 1.0mm, and specific area is 25m
2/ g.
Embodiment 9:
A: adopt dianhydride PMDA and diamines ODA/PPD/OTOL synthesize and be prepared into polyimide fiber, cut into through cutting mechanics the staple fibre that length is 60mm, be then dispersed in water the suspension being made into 1%;
B: suspension is discongested through disc mill, cut off, brooming 40min, makes the slurry that average single fiber length is 3.7mm, fully fibrillation;
C: the KOH alkaline solution treatment 10 minutes that through dehydration, slurry enters that concentration is 0.5mol/L, temperature is 25 DEG C, after dehydrate after fully washing.
D: dried slurry is made loose polyimides pulp after fibrillation loosens process, the specific area of pulp is 6m
2/ g.
According to polyimides pulp prepared by the method, the average length of described pulp fibers is 3.7mm, and specific area is 6m
2/ g.
Embodiment 10:
A: adopt dianhydride ODPA and α-BPDA and diamines TFDB and MPD synthesize and be prepared into polyimide fiber, cut into through cutting mechanics the staple fibre that length is 25mm, be then dispersed in water the suspension being made into 20%;
B: suspension is discongested through disc mill, cut off, brooming 115min, makes the slurry that average single fiber length is 1.5mm, fully fibrillation;
C: the high temperature NaOH alkaline solution treatment 2 minutes that through dehydration, slurry enters that concentration is 6mol/L, temperature is 80 DEG C, after dehydrate after fully washing.
D: dried slurry is made loose polyimides pulp after fibrillation loosens process, the specific area of pulp is 8m
2/ g.
According to polyimides pulp prepared by the method, the average length of described pulp fibers is 1.5mm, and specific area is 8m
2/ g.
Embodiment 11:
A: adopt dianhydride PMDA and diamines ODA and PPD synthesize and be prepared into polyimide fiber, cut into through cutting mechanics the staple fibre that length is 6mm, be then dispersed in water the suspension being made into 17%;
B: suspension is discongested through disc mill, cut off, brooming 40min, makes the slurry that average single fiber length is 0.7mm, fully fibrillation;
C: the KOH alkaline solution treatment 70 minutes that through dehydration, slurry enters that concentration is 3mol/L, temperature is 60 DEG C, after dehydrate after fully washing.
D: dried slurry is made loose polyimides pulp after fibrillation loosens process, the specific area of pulp is 17m
2/ g.
According to polyimides pulp prepared by the method, the average length of described pulp fibers is 0.7mm, and specific area is 17m
2/ g.
Embodiment 12:
A: adopt dianhydride BPDA and PMDA and diamines ODA/MPD/AAQ synthesize and be prepared into polyimide fiber, cut into through cutting mechanics the staple fibre that length is 2mm, be then dispersed in water the suspension being made into 0.3%;
B: suspension is discongested through disc mill, cut off, brooming 70min, makes the slurry that average single fiber length is 0.6mm, fully fibrillation;
C: the NaOH alkaline solution treatment 100 minutes that through dehydration, slurry enters that concentration is 7mol/L, temperature is 45 DEG C, after dehydrate after fully washing.
D: dried slurry is made loose polyimides pulp after fibrillation loosens process, the specific area of pulp is 15m
2/ g.
According to polyimides pulp prepared by the method, the average length of described pulp fibers is 0.6mm, and specific area is 15m
2/ g.
Last it is noted that above embodiment only in order to illustrate the present invention and and unrestricted technical scheme described in the invention; Therefore, although this description reference the above embodiments are to present invention has been detailed description, but, those of ordinary skill in the art is to be understood that, still can modify to the present invention or equivalent replacement: and all do not depart from technical scheme and the tool improvement of the spirit and scope of invention, it all should be encompassed in the middle of right of the present invention.
Claims (6)
1. a preparation method for polyimides (PI) pulp, is characterized in that, comprise the following steps:
A: the polyimide fiber that is prepared into will be synthesized by aromatic dianhydride and aromatic diamine to cut into through cutting mechanics the short fiber of 2-30mm, and then be dispersed in water the suspension being made into 0.1%-20%;
B: suspension is discongested through disc mill, cut off, brooming 5-120min, makes the slurry of the abundant fibrillation of single fiber length 0.2-5mm;
C: slurry enters that concentration is 0.1-10mol/L, temperature is process 2-120 minute in the alkali lye of 5-80 DEG C after dehydration, after dehydrate after fully washing;
D: dried slurry is made loose polyimides pulp after fibrillation loosens process, the specific area of pulp is 3-25m/g.
2. preparation method as claimed in claim 1, it is characterized in that, the structural formula of the dianhydride adopted in steps A is aromatic dianhydride, includes but not limited to one or more in following structural:
3. preparation method as claimed in claim 1, it is characterized in that, the structural formula of the diamines adopted in steps A is aromatic diamines, includes but not limited to one or more in following structural:
4. preparation method as claimed in claim 1, it is characterized in that, the alkali lye adopted in step C is NaOH or the KOH aqueous solution, and the concentration of solution is 1-8mol/L.
5. preparation method as claimed in claim 1, it is characterized in that, in step C, the processing time of slurry in alkali lye is 20 1 80 minutes, and the temperature of alkali lye is 20-60 DEG C.
6. preparation method as claimed in claim 1 prepares polyimides pulp.
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Cited By (9)
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| CN107034541A (en) * | 2017-04-13 | 2017-08-11 | 江苏先诺新材料科技有限公司 | A kind of halogen-free flameproof fibrous material of resistance to ablation and its preparation method and application |
| CN107434889A (en) * | 2017-09-20 | 2017-12-05 | 西安近代化学研究所 | A kind of low cigarette EPDM clad |
| WO2018027096A1 (en) * | 2016-08-04 | 2018-02-08 | Tetramer Technologies, Llc | Copolymers exhibiting improved thermo-oxidative stability |
| CN107675288A (en) * | 2017-10-19 | 2018-02-09 | 长春高琦聚酰亚胺材料有限公司 | A kind of polyimides superbhort fiber and preparation method thereof |
| CN110528272A (en) * | 2019-09-16 | 2019-12-03 | 武汉纺织大学 | A kind of polyimide fiber fibrillation treatment method |
| JP2020169323A (en) * | 2017-02-23 | 2020-10-15 | 旭化成株式会社 | Composition, composite membrane, and membrane electrode assembly |
| CN111961203A (en) * | 2020-08-11 | 2020-11-20 | 江苏奥神新材料股份有限公司 | Preparation method of modified polyimide pulp |
| CN114573811A (en) * | 2021-12-29 | 2022-06-03 | 宁波博雅聚力新材料科技有限公司 | Imide slurry, synthesis method thereof and composition containing imide slurry |
| CN114920974A (en) * | 2022-06-28 | 2022-08-19 | 陕西科技大学 | Cyclic regeneration method of polyimide sponge |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN111961203A (en) * | 2020-08-11 | 2020-11-20 | 江苏奥神新材料股份有限公司 | Preparation method of modified polyimide pulp |
| CN114573811A (en) * | 2021-12-29 | 2022-06-03 | 宁波博雅聚力新材料科技有限公司 | Imide slurry, synthesis method thereof and composition containing imide slurry |
| CN114573811B (en) * | 2021-12-29 | 2023-12-22 | 宁波博雅聚力新材料科技有限公司 | Imide slurry, synthesis method thereof and composition containing imide slurry |
| CN114920974A (en) * | 2022-06-28 | 2022-08-19 | 陕西科技大学 | Cyclic regeneration method of polyimide sponge |
| CN114920974B (en) * | 2022-06-28 | 2023-08-15 | 陕西科技大学 | Recycling method of polyimide sponge |
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