CN106280443A - A kind of composite polyimide material preparation method of high temperature resistant PTFE micropowder - Google Patents
A kind of composite polyimide material preparation method of high temperature resistant PTFE micropowder Download PDFInfo
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- CN106280443A CN106280443A CN201610632339.2A CN201610632339A CN106280443A CN 106280443 A CN106280443 A CN 106280443A CN 201610632339 A CN201610632339 A CN 201610632339A CN 106280443 A CN106280443 A CN 106280443A
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- ptfe micropowder
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- high temperature
- temperature resistant
- polyimide material
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L79/00—Compositions of macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing nitrogen with or without oxygen or carbon only, not provided for in groups C08L61/00 - C08L77/00
- C08L79/04—Polycondensates having nitrogen-containing heterocyclic rings in the main chain; Polyhydrazides; Polyamide acids or similar polyimide precursors
- C08L79/08—Polyimides; Polyester-imides; Polyamide-imides; Polyamide acids or similar polyimide precursors
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J3/00—Processes of treating or compounding macromolecular substances
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2327/00—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Derivatives of such polymers
- C08J2327/02—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Derivatives of such polymers not modified by chemical after-treatment
- C08J2327/12—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Derivatives of such polymers not modified by chemical after-treatment containing fluorine atoms
- C08J2327/18—Homopolymers or copolymers of tetrafluoroethylene
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/08—Stabilised against heat, light or radiation or oxydation
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- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
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- Processes Of Treating Macromolecular Substances (AREA)
- Compositions Of Macromolecular Compounds (AREA)
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Abstract
The invention discloses a kind of composite polyimide material preparation method with high temperature resistant PTFE micropowder, comprise the steps: to put in the reactor with agitator by PTFE micropowder, replace through nitrogen, evacuation, repeatedly after 3～5 times, the mixed gas of fluorine gas and nitrogen it is passed through in reactor, under 20～80rpm stir speed (S.S.)s, reactor is risen to heating-up temperature 100 DEG C～200 DEG C, it is down to 25 DEG C after process time 10min～2h, nitrogen metathesis reactor, PTFE micropowder is after crushed, it is thus achieved that composite polyimide material is with high temperature resistant PTFE micropowder.Present invention process is simple, it is thus achieved that product there is the advantage of high thermal stability, composite polyimide material application can be met.
Description
Technical field
The present invention relates to field of polymer technology, be specifically related to a kind of composite polyimide material system with high temperature resistant PTFE micropowder
Preparation Method.
Background technology
TPI is the thermoplastic polyester in molecule structure containing imide group.Because of it
There is mechanical property, dielectric properties and the moisture-proof of excellence, wear-resisting, radiation hardness and the plurality of advantages such as corrosion-resistant.Automobile, communication,
There is purposes widely the high-end fields such as machinery, electronics, Aero-Space, nuclear power, track traffic, aircraft, new forms of energy.And pure heat
Plastic polyimide is the most poor in processing characteristics, needs to add certain auxiliary agent (such as PTFE micropowder) and improves its processing characteristics,
The friction and wear behavior of polyimide resin can also be improved simultaneously.Because of the special molecular structure of polyimides, its processing temperature exists
380 DEG C～410 DEG C, and the PTFE micropowder that traditional method prepares can thermally decompose at the temperature disclosed above, affects polyimides multiple
The performance of combination product.Therefore, it is badly in need of finding the preparation of the PTFE micropowder that a kind of technique is simple, heat decomposition temperature meets above-mentioned requirements
Method.
Summary of the invention
Present invention aim at solving above-mentioned technical problem present in prior art, it is provided that a kind of polyimides composite wood
The material preparation method of high temperature resistant PTFE micropowder, technique is simple, easily realizes industrialization, it is thus achieved that PTFE micropowder initial pyrolyzation temperature
More than 400 DEG C, the advantage with high thermal stability, can prepare as composite polyimide material, be applied to Aero-Space, vapour
The fields such as car.
In order to solve above-mentioned technical problem, the present invention adopts the following technical scheme that
A kind of composite polyimide material preparation method of high temperature resistant PTFE micropowder, it is characterised in that include walking as follows
Rapid: PTFE micropowder is put in the reactor with agitator, replace through nitrogen, evacuation, repeatedly after 3～5 times, to reactor
In be passed through the mixed gas of fluorine gas and nitrogen, under 20～80rpm stir speed (S.S.)s, reactor is risen to heating-up temperature 100 DEG C～
200 DEG C, being down to 25 DEG C after processing time 10min～2h, nitrogen metathesis reactor, PTFE micropowder is after crushed, it is thus achieved that polyamides is sub-
Amine composite is with high temperature resistant PTFE micropowder；This preparation method technique is simple, it is thus achieved that product there is the advantage of high thermal stability,
Composite polyimide material application can be met.
Further, the mean diameter of PTFE micropowder is 0.5～10 μm, and preferably 1～5 μm, by irradiation, thermal cracking, suspension
A kind of preparation method of polymerization or emulsion polymerization obtains.The implementation result of the present invention is relevant with the mean diameter of PTFE micropowder, shadow
Ring to process time and fluorine gas, the volume ratio of nitrogen mixed gas.Mean diameter is the least, and PTFE micropowder bulk density is too big, place
The reason time is oversize, affects implementation result；Mean diameter is too big, and it is long that fluorine gas penetrates into the PTFE micropowder internal layer time, during the process of needs
Between oversize, affect implementation result.
Further, in mixed gas, the volume ratio of fluorine gas and nitrogen is 1:1～1:10, preferably 1:2～1:4, the present invention's
Implementation result is relevant with the volume ratio of fluorine gas, nitrogen mixed gas, has influence on the process time, and volume ratio is the least, processes the time too
Long, affect implementation result；Volume ratio is too big, requires the highest to process safety.
Further, stir speed (S.S.) preferably 30～50rpm, the implementation result of the present invention is relevant with stir speed (S.S.), stir speed (S.S.)
The lowest, process the time oversize, affect implementation result；Stir speed (S.S.) is the highest, requires the highest to process safety.
Further, heating-up temperature preferably 120 DEG C～170 DEG C, the implementation result of the present invention is relevant with heating-up temperature, heating temperature
Spend the lowest, process the time oversize, affect implementation result；Heating-up temperature is the highest, and PTFE micropowder easily occurs irreversible adhesion.
Further, the process time is 1h～1.5h, and the implementation result of the present invention is relevant with the time of process, processes the time too
Short, affect implementation result；The process time is oversize, affects production efficiency, and PTFE micropowder easily occurs irreversible adhesion.
Due to the fact that and have employed technique scheme, have the advantages that
The present invention uses the gaseous mixture of fluorine gas and nitrogen to be processing mode, and technique is simple, easily realizes industrialization, it is thus achieved that PTFE
Micropowder initial pyrolyzation temperature is (untreated PTFE micropowder initial pyrolyzation temperature is 361 DEG C～366 DEG C) more than 400 DEG C,
The advantage with high thermal stability, can prepare as composite polyimide material, is applied to the field such as Aero-Space, automobile.
Detailed description of the invention
A kind of composite polyimide material of present invention preparation method of high temperature resistant PTFE micropowder, comprise the steps: by
PTFE micropowder is put in the reactor with agitator, and reactor is that design pressure is more than or equal to the vertical retort of 0.1MPa or horizontal
The one of still, agitator is magnetic agitation or churned mechanically one, and the mean diameter of PTFE micropowder is 0.5～10 μm, preferably 1
～5 μm, obtained by a kind of preparation method of irradiation, thermal cracking, suspension polymerisation or emulsion polymerization.The implementation result of the present invention with
The mean diameter of PTFE micropowder is relevant, has influence on process time and fluorine gas, the volume ratio of nitrogen mixed gas.Mean diameter is too
Little, PTFE micropowder bulk density is too big, processes the time oversize, affects implementation result；Mean diameter is too big, and it is micro-that fluorine gas penetrates into PTFE
The powder internal layer time is long, and the process time of needs is oversize, affects implementation result.Replace through nitrogen, evacuation, repeatedly after 3～5 times,
Being passed through the mixed gas of fluorine gas and nitrogen in reactor, in mixed gas, the volume ratio of fluorine gas and nitrogen is 1:1～1:10, excellent
Selecting 1:2～1:4, the implementation result of the present invention is relevant with the volume ratio of fluorine gas, nitrogen mixed gas, has influence on process time, body
Long-pending ratio is the least, processes the time oversize, affects implementation result；Volume ratio is too big, requires the highest to process safety.
Under 30～50rpm stir speed (S.S.)s, reactor is risen to heating-up temperature 120 DEG C～170 DEG C, process time 1h～
Being down to 25 DEG C after 1.5h, nitrogen metathesis reactor, PTFE micropowder is after crushed, it is thus achieved that composite polyimide material is with high temperature resistant
PTFE micropowder.The implementation result of the present invention is relevant with stir speed (S.S.), and stir speed (S.S.) is the lowest, processes the time oversize, and effect is implemented in impact
Really；Stir speed (S.S.) is the highest, requires the highest to process safety.The implementation result of the present invention is relevant with heating-up temperature, and heating-up temperature is too
Low, process the time oversize, affect implementation result；Heating-up temperature is the highest, and PTFE micropowder easily occurs irreversible adhesion.The reality of the present invention
Execute effect relevant with the process time, process the time the shortest, affect implementation result；The process time is oversize, affects production efficiency, PTFE
Easily there is irreversible adhesion in micropowder.
The present invention uses the gaseous mixture of fluorine gas and nitrogen to be processing mode, and technique is simple, easily realizes industrialization, it is thus achieved that PTFE
Micropowder initial pyrolyzation temperature is (untreated PTFE micropowder initial pyrolyzation temperature is 361 DEG C～366 DEG C) more than 400 DEG C,
The advantage with high thermal stability, can prepare as composite polyimide material, is applied to the field such as Aero-Space, automobile.
Embodiment 1
The PTFE micropowder 10kg that mean diameter is 0.5 μm is put in the 50L reactor with agitator, puts through nitrogen
Change, evacuation, repeatedly after 3 times, in reactor, be passed through fluorine gas and nitrogen mixed gas that volume ratio is 1:10, stir at 20rpm
Mixing under speed, reactor rises to heating-up temperature 100 DEG C, the process time is to be down to 25 DEG C after 2h, nitrogen metathesis reactor, PTFE
Micropowder is after crushed, it is thus achieved that composite polyimide material is 405 DEG C with high temperature resistant PTFE micropowder, initial pyrolyzation temperature.
Embodiment 2
The PTFE micropowder 10kg that mean diameter is 10 μm is put in the 50L reactor with agitator, replaces through nitrogen,
Evacuation, repeatedly after 5 times, is passed through fluorine gas and nitrogen mixed gas that volume ratio is 1:1 in reactor, in 80rpm stirring speed
Under rate, reactor rising to heating-up temperature 200 DEG C, the process time is to be down to 25 DEG C after 30min, nitrogen metathesis reactor, PTFE
Micropowder is after crushed, it is thus achieved that composite polyimide material is 401 DEG C with high temperature resistant PTFE micropowder, initial pyrolyzation temperature.
Embodiment 3
The PTFE micropowder 10kg that mean diameter is 1 μm is put in the 50L reactor with agitator, replaces through nitrogen,
Evacuation, repeatedly after 5 times, is passed through fluorine gas and nitrogen mixed gas that volume ratio is 1:3 in reactor, in 30rpm stirring speed
Under rate, reactor rising to heating-up temperature 200 DEG C, the process time is to be down to 25 DEG C after 30min, nitrogen metathesis reactor, PTFE
Micropowder is after crushed, it is thus achieved that composite polyimide material is 407 DEG C with high temperature resistant PTFE micropowder, initial pyrolyzation temperature.
Embodiment 4
The PTFE micropowder 10kg that mean diameter is 3 μm is put in the 50L reactor with agitator, replaces through nitrogen,
Evacuation, repeatedly after 5 times, is passed through fluorine gas and nitrogen mixed gas that volume ratio is 1:5 in reactor, in 40rpm stirring speed
Under rate, reactor rising to heating-up temperature 120 DEG C, the process time is to be down to 25 DEG C after 1.5h, and nitrogen metathesis reactor, PTFE is micro-
Powder is after crushed, it is thus achieved that composite polyimide material is 410 DEG C with high temperature resistant PTFE micropowder, initial pyrolyzation temperature.
Embodiment 5
The PTFE micropowder 10kg that mean diameter is 5 μm is put in the 50L reactor with agitator, replaces through nitrogen,
Evacuation, repeatedly after 5 times, is passed through fluorine gas and nitrogen mixed gas that volume ratio is 1:7 in reactor, in 50rpm stirring speed
Under rate, reactor rising to heating-up temperature 170 DEG C, the process time is to be down to 25 DEG C after 1h, nitrogen metathesis reactor, PTFE micropowder
After crushed, it is thus achieved that composite polyimide material is 408 DEG C with high temperature resistant PTFE micropowder, initial pyrolyzation temperature.
These are only the specific embodiment of the present invention, but the technical characteristic of the present invention is not limited thereto.Any with this
Based on bright, for solving essentially identical technical problem, it is achieved essentially identical technique effect, done simple change, etc.
With replacement or modification etc., all it is covered by among protection scope of the present invention.
Claims (6)
1. the composite polyimide material preparation method of high temperature resistant PTFE micropowder, it is characterised in that comprise the steps:
PTFE micropowder is put in the reactor with agitator, replaces through nitrogen, evacuation, repeatedly after 3～5 times, in reactor
It is passed through the mixed gas of fluorine gas and nitrogen, under 20～80rpm stir speed (S.S.)s, reactor is risen to heating-up temperature 100 DEG C～200
DEG C, it is down to 25 DEG C after processing time 10min～2h, nitrogen metathesis reactor, PTFE micropowder is after crushed, it is thus achieved that polyimides is multiple
Condensation material is with high temperature resistant PTFE micropowder.
A kind of composite polyimide material the most according to claim 1 preparation method of high temperature resistant PTFE micropowder, it is special
Levy and be: the mean diameter of described PTFE micropowder is 0.5～10 μm, preferably 1～5 μm.
A kind of composite polyimide material the most according to claim 1 preparation method of high temperature resistant PTFE micropowder, it is special
Levy and be: in described mixed gas, the volume ratio of fluorine gas and nitrogen is 1:1～1:10, preferably 1:2～1:4.
A kind of composite polyimide material the most according to claim 1 preparation method of high temperature resistant PTFE micropowder, it is special
Levy and be: described stir speed (S.S.) preferably 30～50rpm.
A kind of composite polyimide material the most according to claim 1 preparation method of high temperature resistant PTFE micropowder, it is special
Levy and be: described heating-up temperature preferably 120 DEG C～170 DEG C.
A kind of composite polyimide material the most according to claim 1 preparation method of high temperature resistant PTFE micropowder, it is special
Levy and be: the described process time is 1h～1.5h.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201610632339.2A CN106280443A (en) | 2016-08-02 | 2016-08-02 | A kind of composite polyimide material preparation method of high temperature resistant PTFE micropowder |
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| CN201610632339.2A CN106280443A (en) | 2016-08-02 | 2016-08-02 | A kind of composite polyimide material preparation method of high temperature resistant PTFE micropowder |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20210040303A1 (en) * | 2018-02-07 | 2021-02-11 | Daiking Industries, Ltd | Method for producing composition containing low molecular weight polytetrafluoroethylene |
Citations (2)
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|---|---|---|---|---|
| US20080187848A1 (en) * | 2006-10-05 | 2008-08-07 | Konica Minolta Business Technologies, Inc. | Electrophotographic Photoreceptor, and Process Cartridge and Image Forming Apparatus Employing the Same |
| CN103665215A (en) * | 2013-11-29 | 2014-03-26 | 中昊晨光化工研究院有限公司 | PTFE suspension resin end group fluorination treatment method |
-
2016
- 2016-08-02 CN CN201610632339.2A patent/CN106280443A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20080187848A1 (en) * | 2006-10-05 | 2008-08-07 | Konica Minolta Business Technologies, Inc. | Electrophotographic Photoreceptor, and Process Cartridge and Image Forming Apparatus Employing the Same |
| CN103665215A (en) * | 2013-11-29 | 2014-03-26 | 中昊晨光化工研究院有限公司 | PTFE suspension resin end group fluorination treatment method |
Non-Patent Citations (2)
| Title |
|---|
| JAE-HO KIM ET AL.,: "Improved thermal stability of crosslinked PTFE using fluorine gas treatment", 《JOURNAL OF FLUORINE CHEMISTRY》 * |
| 汪星平 等: "含氟聚合物不稳定端基形成机理及其稳定化处理", 《化工生产与技术》 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20210040303A1 (en) * | 2018-02-07 | 2021-02-11 | Daiking Industries, Ltd | Method for producing composition containing low molecular weight polytetrafluoroethylene |
| US11739205B2 (en) * | 2018-02-07 | 2023-08-29 | Daikin Industries, Ltd. | Method for producing composition containing low molecular weight polytetrafluoroethylene |
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