CN104974522A - Preparation of polyimide high-temperature-resistant composite material surrounding airplane engine - Google Patents
Preparation of polyimide high-temperature-resistant composite material surrounding airplane engine Download PDFInfo
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- CN104974522A CN104974522A CN201410144739.XA CN201410144739A CN104974522A CN 104974522 A CN104974522 A CN 104974522A CN 201410144739 A CN201410144739 A CN 201410144739A CN 104974522 A CN104974522 A CN 104974522A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K7/00—Use of ingredients characterised by shape
- C08K7/02—Fibres or whiskers
- C08K7/04—Fibres or whiskers inorganic
- C08K7/14—Glass
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C70/00—Shaping composites, i.e. plastics material comprising reinforcements, fillers or preformed parts, e.g. inserts
- B29C70/04—Shaping composites, i.e. plastics material comprising reinforcements, fillers or preformed parts, e.g. inserts comprising reinforcements only, e.g. self-reinforcing plastics
- B29C70/28—Shaping operations therefor
- B29C70/54—Component parts, details or accessories; Auxiliary operations, e.g. feeding or storage of prepregs or SMC after impregnation or during ageing
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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
- C08J5/00—Manufacture of articles or shaped materials containing macromolecular substances
- C08J5/04—Reinforcing macromolecular compounds with loose or coherent fibrous material
- C08J5/0405—Reinforcing macromolecular compounds with loose or coherent fibrous material with inorganic fibres
- C08J5/043—Reinforcing macromolecular compounds with loose or coherent fibrous material with inorganic fibres with glass fibres
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/30—Sulfur-, selenium- or tellurium-containing compounds
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K5/00—Use of organic ingredients
- C08K5/49—Phosphorus-containing compounds
- C08K5/51—Phosphorus bound to oxygen
- C08K5/52—Phosphorus bound to oxygen only
- C08K5/524—Esters of phosphorous acids, e.g. of H3PO3
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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
- C08J2379/00—Characterised by the use 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 C08J2361/00 - C08J2377/00
- C08J2379/04—Polycondensates having nitrogen-containing heterocyclic rings in the main chain; Polyhydrazides; Polyamide acids or similar polyimide precursors
- C08J2379/08—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
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/30—Sulfur-, selenium- or tellurium-containing compounds
- C08K2003/3045—Sulfates
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- Engineering & Computer Science (AREA)
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- Manufacturing & Machinery (AREA)
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- Composite Materials (AREA)
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Abstract
The invention provides a polyimide high-temperature-resistant composite material surrounding an airplane engine and a preparation method thereof, wherein the composite material includes following components, by mass, 70-90% of polyimide, 10-30% of short-cut glass fibers, 0.2-0.6% of a thermal stabilizer (tribasic lead sulfate), and 0.1-0.3% of an anti-oxidant (trisnonylphenyl phosphate, TNP). The preparation method includes following steps: (1) drying the polyimide resin at 150-175 DEG C; (2) blending the polyimide resin, the thermal stabilizer and the anti-oxidant; (3) feeding the blended material into a double-screw extruder and performing melting extrusion through a special die head at a processing temperature of 390-410 DEG C; (4) pre-heating and drying continuous glass fibers, mixing the continuous glass fibers with the molten resin in the die head through a special die head, wherein the continuous glass fiber bundles are completely impregnated with the molten resin through a certain distance in the die head, and at the same time the glass fiber bundles and the molten resin are extruded from the mouth of the special die head; and (5) finally cooling, drying and pelletizing the extruded semi-product to obtain the continuously-glass-fiber-reinforced polyimide material. The preparation method is simple in process. The production devices are easy to operate. The composite material is excellent in performance.
Description
Technical field
The present invention relates to a kind of glass fiber reinforced polyester imide high temperature resistant composite, particularly continuous glass fibre strengthens polyimide material and preparation method thereof, belongs to polymeric material field.
Background technology
Polyimide is the macromolecular material containing imide ring on a class main chain.Due to main chain containing aromatic nucleus, it is as advanced composite material matrix, and having outstanding heat resistance and excellent mechanical property, is one of material that in current polymer matrix composites, temperature tolerance is the highest.
This project uses thermoplastic polyimide resin to be matrix, by by itself and glass fibre compound, prepare 200 degrees Celsius of lower rigidity and reduce by 20% more than PEEK 3 times, thermal expansivity, it is the ideal material of alternative metal under specified conditions, pottery, thermosetting resin, lower temperature thermoplastics and unmanageable polyimide, for the alloy material of the high temperature resistant oil and gas environments such as aircraft engine machine bearing and bearing shell, engine weight can be alleviated and improve engine thrust-weight ratio.Use heat plastic resin prepares aircraft engine component, than metallic substance and thermosetting material design and shaping more convenient; These component can anti-electrostatic, can with metallic contact; There is certain flame retardant resistance.
Summary of the invention
Due to the glass fiber reinforced polyester imide material adopting conventional machining process to produce, the length-to-diameter ratio of glass fibre in resin is less than normal, and length distribution range is larger, cause the reinforced effects of glass fibre in resin not to be not fully exerted, its application in modified plastics is restricted.The invention provides the preparation method that a kind of continuous glass fibre strengthens polyimide material, effectively increase the length-to-diameter ratio of glass fibre in resin, substantially increase the mechanical property of material.
preparation method of the present invention comprises the following steps:
(1), polyimide resin is carried out drying and processing under 150 ~ 175 DEG C of conditions;
(2), starting material polyimide resin, thermo-stabilizer, oxidation inhibitor are joined in mixing machine by prescription quality percentage, carry out Homogeneous phase mixing at normal temperatures;
(3), by above-mentioned mixed material join in forcing machine charging basket, melt extruded by twin screw extruder.Extruder barrel processing temperature is set as 390 ~ 410 DEG C, and main-machine screw rotating speed is 220 ~ 250r.min
-1, main feeding rotating speed is 10 ~ 18r.min
-1;
(4), by continuous glass fibre bundle first carry out drying treatment by open type baking oven, oven temperature is 90 ~ 100 DEG C, then continuous glass fibre is passed from special extruder die head, and forcing machine starts to melt extrude simultaneously.In die head, the resin of continuous glass fibre and complete melting converges, and continuous glass fibre is completely infused in molten resin by scattered by force in die head simultaneously.The roving glass fiber completely coated by resin melt is pulled out by from die head, cools through air cooling equipment, under the traction of tractor, material strip is sent in dicing machine and carries out pelletizing, namely generates continuous glass fibre and strengthens polyimide material.
Below by specific embodiment, patent of the present invention is specifically described:
embodiment 1:
According to mass percent, by 70 parts of linear polyimide resins, 0.2 part of thermo-stabilizer (tribasic lead sulfate), 0.1 part of oxidation inhibitor (tris phosphite TNP) carries out Homogeneous phase mixing jointly in mixing machine, is then poured in forcing machine charging basket by mixture.30 parts of continuous continuous glass fibres by oven drying process, oven temperature is 100 DEG C, then continuous glass fibre is passed from extruder die head, opens forcing machine simultaneously.Extruder barrel processing temperature is 390 ~ 410 DEG C, forcing machine establishes eight sections altogether, first paragraph and second segment are 390 DEG C, 3rd section and the 4th section is 395 DEG C, and other several sections is 410 DEG C, and main-machine screw rotating speed is 220r.min-1, main feeding rotating speed is 10r.min-1, molten resin is extruded after continuous glass fibre thorough impregnation from die head in die head, then through overcooling, air-dry, traction, is finally cut into the particle that length is 5mm.
embodiment 2:
According to mass percent, by 70 parts of linear polyimide resins, 0.2 part of thermo-stabilizer (tribasic lead sulfate), 0.1 part of oxidation inhibitor (tris phosphite TNP) carries out Homogeneous phase mixing jointly in mixing machine, is then poured in forcing machine charging basket by mixture.30 parts of continuous continuous glass fibres by oven drying process, oven temperature is 100 DEG C, then continuous glass fibre is passed from extruder die head, opens forcing machine simultaneously.Extruder barrel processing temperature is 390 ~ 410 DEG C, forcing machine establishes eight sections altogether, first paragraph and second segment are 390 DEG C, 3rd section and the 4th section is 395 DEG C, and other several sections is 410 DEG C, and main-machine screw rotating speed is 220r.min-1, main feeding rotating speed is 10r.min-1, molten resin is extruded after continuous glass fibre thorough impregnation from die head in die head, then through overcooling, air-dry, traction, is finally cut into the particle that length is 8mm.
embodiment 3:
According to mass percent, by 70 parts of linear polyimide resins, 0.2 part of thermo-stabilizer (tribasic lead sulfate), 0.1 part of oxidation inhibitor (tris phosphite TNP) carries out Homogeneous phase mixing jointly in mixing machine, is then poured in forcing machine charging basket by mixture.30 parts of continuous continuous glass fibres by oven drying process, oven temperature is 100 DEG C, then continuous glass fibre is passed from extruder die head, opens forcing machine simultaneously.Extruder barrel processing temperature is 390 ~ 410 DEG C, forcing machine establishes eight sections altogether, first paragraph and second segment are 390 DEG C, 3rd section and the 4th section is 395 DEG C, and other several sections is 410 DEG C, and main-machine screw rotating speed is 220r.min-1, main feeding rotating speed is 10r.min-1, molten resin is extruded after continuous glass fibre thorough impregnation from die head in die head, then through overcooling, air-dry, traction, is finally cut into the particle that length is 11mm.
embodiment 4:
According to mass percent, by 70 parts of linear polyimide resins, 0.2 part of thermo-stabilizer (tribasic lead sulfate), 0.1 part of oxidation inhibitor (tris phosphite TNP) carries out Homogeneous phase mixing jointly in mixing machine, is then poured in forcing machine charging basket by mixture.30 parts of continuous continuous glass fibres by oven drying process, oven temperature is 100 DEG C, then continuous glass fibre is passed from extruder die head, opens forcing machine simultaneously.Extruder barrel processing temperature is 390 ~ 410 DEG C, forcing machine establishes eight sections altogether, first paragraph and second segment are 390 DEG C, 3rd section and the 4th section is 395 DEG C, and other several sections is 410 DEG C, and main-machine screw rotating speed is 220r.min-1, main feeding rotating speed is 10r.min-1, molten resin is extruded after continuous glass fibre thorough impregnation from die head in die head, then through overcooling, air-dry, traction, is finally cut into the particle that length is 14mm.
embodiment 5:
According to mass percent, by 70 parts of linear polyimide resins, 0.2 part of thermo-stabilizer (tribasic lead sulfate), 0.1 part of oxidation inhibitor (tris phosphite TNP) carries out Homogeneous phase mixing jointly in mixing machine, is then poured in forcing machine charging basket by mixture.30 parts of continuous continuous glass fibres by oven drying process, oven temperature is 100 DEG C, then continuous glass fibre is passed from extruder die head, opens forcing machine simultaneously.Extruder barrel processing temperature is 390 ~ 410 DEG C, forcing machine establishes eight sections altogether, first paragraph and second segment are 390 DEG C, 3rd section and the 4th section is 395 DEG C, and other several sections is 410 DEG C, and main-machine screw rotating speed is 220r.min-1, main feeding rotating speed is 10r.min-1, molten resin is extruded after continuous glass fibre thorough impregnation from die head in die head, then through overcooling, air-dry, traction, is finally cut into the particle that length is 17mm.
embodiment 6:
According to mass percent, by 70 parts of linear polyimide resins, 0.2 part of thermo-stabilizer (tribasic lead sulfate), 0.1 part of oxidation inhibitor (tris phosphite TNP) carries out Homogeneous phase mixing jointly in mixing machine, is then poured in forcing machine charging basket by mixture.30 parts of continuous continuous glass fibres by oven drying process, oven temperature is 100 DEG C, then continuous glass fibre is passed from extruder die head, opens forcing machine simultaneously.Extruder barrel processing temperature is 390 ~ 410 DEG C, forcing machine establishes eight sections altogether, first paragraph and second segment are 390 DEG C, 3rd section and the 4th section is 395 DEG C, and other several sections is 410 DEG C, and main-machine screw rotating speed is 220r.min-1, main feeding rotating speed is 10r.min-1, molten resin is extruded after continuous glass fibre thorough impregnation from die head in die head, then through overcooling, air-dry, traction, is finally cut into the particle that length is 20mm.
by product obtained for above six examples with reference to GB/T 17037.1-1997 injection moulding, obtain master body.
material detects by following standard: the results are shown in Table 1.
Table 1: example 1,2,3,4,5,6 product mechanical property and conservation rates thereof
Claims (5)
1. a continuous glass fibre strengthens polyimide material, be primarily characterized in that the mass percentage of each component in formula system is: polyimide 40 ~ 70wt%, the thermo-stabilizer of glass fibre 30 ~ 60wt%, 0.2 ~ 0.6wt%, the oxidation inhibitor of 0.1 ~ 0.3wt%.
2. a kind of continuous glass fibre according to claim 1 strengthens polyimide material, it is characterized in that: the equipment preparing this kind of material is the soak type extruder die head of the special construction of our company's autonomous design, this die head is provided with heating unit, can prevent from reducing molten resin flowing property because die head temperature is low, effectively improve fiber effect of impregnation, solve fiber and infiltrate incomplete phenomenon, fiber orientation is consistent with extruding material strip direction.
3. a kind of continuous glass fibre according to claim 1 strengthens polyimide material, it is characterized in that: described continuous glass fibre diameter is 10 ~ 15 μm, after granulation, glass fibre is isometric with material grain, length is 5 ~ 20mm, fiber effective L D ratio can reach 300 ~ 2000, and fiber is arranged in parallel in the axial direction.
4. a kind of continuous glass fibre according to claim 1 strengthens polyimide material, it is characterized in that: described polyimide is existing commercial linear polyimide resin.
5. a kind of continuous glass fibre according to claim 1 strengthens polyimide material, it is characterized in that: described thermo-stabilizer is tribasic lead sulfate) 0.2 ~ 0.6wt, oxidation inhibitor is tris phosphite TNP.
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Citations (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN1709973A (en) * | 2005-06-30 | 2005-12-21 | 北京航空航天大学 | Inorganic nano combined fiber reinforced polyimide composite material and its preparing method |
US20100108173A1 (en) * | 2008-10-31 | 2010-05-06 | E. I. Du Pont De Nemours And Company | Highly abrasion-resistant polyolefin pipe |
CN101821338A (en) * | 2007-09-10 | 2010-09-01 | 沙伯基础创新塑料知识产权有限公司 | Blow moldable polyimide/polyamide composition, process for blow molding and articles made thereby |
CN102010596A (en) * | 2010-12-27 | 2011-04-13 | 南京立汉化学有限公司 | Glass fibre reinforced polyetherimide and preparation method thereof |
-
2014
- 2014-04-12 CN CN201410144739.XA patent/CN104974522A/en active Pending
Patent Citations (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN1709973A (en) * | 2005-06-30 | 2005-12-21 | 北京航空航天大学 | Inorganic nano combined fiber reinforced polyimide composite material and its preparing method |
CN101821338A (en) * | 2007-09-10 | 2010-09-01 | 沙伯基础创新塑料知识产权有限公司 | Blow moldable polyimide/polyamide composition, process for blow molding and articles made thereby |
US20100108173A1 (en) * | 2008-10-31 | 2010-05-06 | E. I. Du Pont De Nemours And Company | Highly abrasion-resistant polyolefin pipe |
CN102010596A (en) * | 2010-12-27 | 2011-04-13 | 南京立汉化学有限公司 | Glass fibre reinforced polyetherimide and preparation method thereof |
Non-Patent Citations (1)
Title |
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徐同考: "《塑料改性实用技术》", 30 June 2012 * |
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