CN103756313A - Method used for increasing hear resistance of ketone-anhydride type polyimide retainer tube blank - Google Patents
Method used for increasing hear resistance of ketone-anhydride type polyimide retainer tube blank Download PDFInfo
- Publication number
- CN103756313A CN103756313A CN201310683681.1A CN201310683681A CN103756313A CN 103756313 A CN103756313 A CN 103756313A CN 201310683681 A CN201310683681 A CN 201310683681A CN 103756313 A CN103756313 A CN 103756313A
- Authority
- CN
- China
- Prior art keywords
- retainer
- acid anhydride
- anhydride type
- type polyimide
- ether acid
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
Classifications
-
- 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
-
- 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
- B29C71/00—After-treatment of articles without altering their shape; Apparatus therefor
- B29C71/02—Thermal after-treatment
-
- 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
- B29C71/00—After-treatment of articles without altering their shape; Apparatus therefor
- B29C71/02—Thermal after-treatment
- B29C2071/022—Annealing
-
- 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
- C08K2201/00—Specific properties of additives
- C08K2201/002—Physical properties
- C08K2201/003—Additives being defined by their diameter
-
- 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
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2203/00—Applications
- C08L2203/30—Applications used for thermoforming
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/02—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group
- C08L2205/025—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group containing two or more polymers of the same hierarchy C08L, and differing only in parameters such as density, comonomer content, molecular weight, structure
Landscapes
- Chemical & Material Sciences (AREA)
- Physics & Mathematics (AREA)
- Thermal Sciences (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Casting Or Compression Moulding Of Plastics Or The Like (AREA)
- Macromolecular Compounds Obtained By Forming Nitrogen-Containing Linkages In General (AREA)
- Moulding By Coating Moulds (AREA)
Abstract
The invention discloses a method used for increasing hear resistance of ketone-anhydride type polyimide retainer tube blank, and belongs to the field of engineering plastic retainer technology. The method comprises steps of preparation of a retainer tube blank material, drying, mixing, hot press molding, and annealing treatment. According to the method, the retainer tube blank material is subjected to drying and mixing, and then is subjected to hot press molding using a programmed type thermocompressor so as to obtain ketone-anhydride type polyimide composite retainer tube blank; and then the obtained ketone-anhydride type polyimide composite retainer tube blank is subjected to annealing treatment. The obtained ketone-anhydride type polyimide composite retainer tube blank is light, and high temperature tensile strength, tribological properties, and heat resistance are improved effectively.
Description
Technical field
The present invention relates to engineering plastics cage technical field, refer more particularly to a kind of stable on heating method of raising ether acid anhydride type polyimide retainer pipe.
Background technology
Known, ether acid anhydride type polyimide has the advantages such as tensile strength is high, frictional coefficient is little, wear-resistant, especially its forming process is good, be widely used in middle low speed ball bearing retainer field, composite polyimide material retainer has significant material advantage compared with traditional metal alloy retainer promoting aspect the rotating speed of bearing and run stability, is one of important research direction of high temperature and high speed field of bearings.
Conventionally the second-order transition temperature of ether acid anhydride type polyimide is no more than 265 ℃, and heat-drawn wire (1.80MPa) is less than 245 ℃, and Testing Tensile Strength at Elevated Temperature conservation rate is lower, and thermal conductivity is less than 0.2W. (m.K)
-1owing to producing a large amount of heat of friction when the high speed rotating, cannot conduct fast, making retainer surface soften, be out of shape even thermolysis lost efficacy, have a strong impact on bearing operation reliability and life-span, therefore, ether acid anhydride type polyimide thermotolerance deficiency becomes and limits it in the prerequisite of high temperature and high speed retainer field application.
Improving the most basic method of ether acid anhydride type polyimide thermotolerance is the synthetic novel texture polyimide that heat-resisting rank is higher, processing characteristics is good, but this method is subject to the restriction of the factors such as starting material source, synthesis technology, lead time and production cost, and difficulty is excessive, therefore, promote lay particular emphasis on by blend or fill method of the stable on heating research of polyimide more and prepare the more much higher phase-polymerization objects system of thermotolerance, so, Chinese scholars is utilized aramid fiber, copper powder, glass fibre, carbon fiber, potassium titanate crystal whisker and nano material etc. are carried out blend to it, filling-modified, to promoting the thermotolerance of ether acid anhydride type polyimide, yet, the stable on heating lifting of ether acid anhydride type matrix material that this method of modifying is made be take and sacrificed its tensile strength and bring as cost, therefore, it is limited that thermotolerance promotes amplitude, be difficult to meet the demand of high temperature and high speed bearing to retainer material thermal resistance.
The second-order transition temperature of polypyromelliticimide molding powder is greater than 380 ℃, its structure and ether acid anhydride type polyimide are comparatively approaching, good bonding strength between the composite material interface being made by its modification ether acid anhydride type polyimide, tensile strength conservation rate is higher, and thermotolerance is also able to remarkable lifting; Meanwhile, add the thermal conductivity that heat conduction lubricant can improve ether acid anhydride type polyimide, improve its tribological property, at present, the domestic report there is no by polypyromelliticimide molding powder, heat conduction lubricant modification ether acid anhydride type polyimide retainer pipe method.
Summary of the invention
In order to realize described goal of the invention, the invention discloses a kind of stable on heating method of raising ether acid anhydride type polyimide retainer pipe, described method is by being the material of preparing retainer pipe by ether acid anhydride type polyimide molding powder, polypyromelliticimide and heat conduction lubricant, by the material of retainer pipe after drying treatment and proportioning operation on program control type thermocompressor the hot-forming ether acid anhydride type polyimide composite holder pipe that obtains, the ether acid anhydride type polyimide composite holder pipe obtaining is carried out to anneal; Retainer quality of tube blank steel that the present invention produces is light, Testing Tensile Strength at Elevated Temperature is high, tribological property and thermotolerance better.
In order to realize the object solving the problems of the technologies described above, the present invention has adopted following technical scheme:
The stable on heating method of raising ether acid anhydride type polyimide retainer pipe, comprises and prepares retainer blank tube material, drying treatment, proportioning operation, hot-forming and anneal, and its concrete operation step is as follows:
(1) prepare retainer blank tube material:
Retainer blank tube material comprises by weight percentage: 59%～80% ether acid anhydride type polyimide molding powder, 15%～40% polypyromelliticimide and 1%～5% heat conduction lubricant;
(2) drying treatment:
Connect previous step, the retainer blank tube material that previous step is obtained is put into respectively loft drier drying treatment, then crosses respectively 200 mesh sieves independent sealed saving backup;
(3) proportioning operation:
Connect previous step, get respectively by weight percentage dry 59%～80% the ether acid anhydride type polyimide molding powder that obtains in previous step, 15%～40% polypyromelliticimide molding powder and 1%～5% heat conduction lubricant, successively put into machine mixer and stir, make ether acid anhydride type polyimide molding powder matrix material;
(4) hot-forming:
Connect previous step, the ether acid anhydride type polyimide molding powder matrix material that previous step is obtained is filled in retainer mould, then retainer mould is placed on program control type thermocompressor, hot-forming ether acid anhydride type polyimide composite holder pipe;
(5) anneal:
Connect previous step, the ether acid anhydride type polyimide composite holder pipe that previous step is obtained is placed on sintering in sintering oven, the heat-up rate of sintering oven is controlled at 50～70 ℃/h, while being warming up to 150 ℃ in sintering oven, be incubated 2h, then continue when heat-up rate with 12～20 ℃/h is warming up to 280 ℃ to be incubated 8～10h, the speed with 30～40 ℃/h is cooled to 50 ℃ of taking-ups afterwards.
The described stable on heating method of raising ether acid anhydride type polyimide retainer pipe, the ether acid anhydride type polyimide molding powder described in step 1, polypyromelliticimide and the particle diameter of heat conduction lubricant be 200 orders.
The described stable on heating method of raising ether acid anhydride type polyimide retainer pipe, the heat conduction lubricant described in step 1 is at least comprising any in carbon fiber powder, graphite, carbon nanotube.
The described stable on heating method of raising ether acid anhydride type polyimide retainer pipe, the temperature of the drying treatment described in step 2 is 230 ℃, and be 3h time of drying, and dry rear taking-up is cooled to room temperature.
The described stable on heating method of raising ether acid anhydride type polyimide retainer pipe, stirring number of times in proportioning operation described in step 3 is 3～5 times, each time of stirring is controlled at 20～30 seconds, and while stirring, the rotating speed of machine mixer is controlled at 10000～12000 revs/min at every turn.
The described stable on heating method of raising ether acid anhydride type polyimide retainer pipe, is comprised of overcoat, fuse, drift and base four parts at the retainer mould described in hot-forming step, and wherein overcoat, fuse and base form retainer die cavity; In retainer mould, the internal diameter size of overcoat is to increase 3mm on the basis of bearing finished products retainer outside dimension, and in retainer mould, the outside dimension of fuse is to dwindle 3mm on the basis of bearing finished products retainer internal diameter size; In retainer mould, the height dimension of overcoat and fuse is on the basis of bearing finished products retainer height dimension, to increase more than 3 times; In retainer mould, the internal diameter size of drift and the outside dimension of fuse match, and the internal diameter size of described base and the outside dimension of fuse match, and the outside dimension of described base and the internal diameter size of overcoat match.
The described stable on heating method of raising ether acid anhydride type polyimide retainer pipe, in the pressure-controlling of the program control type thermocompressor described in hot-forming step at 300～600kg/cm
2, suppress the air of getting rid of for 5 minutes in retainer mould, after 5 minutes to retainer mold heated, 60 minutes post-heating to 385 ℃, between heating period, pressure-controlling is at 300～600kg/cm
2; When temperature reaches 385 ℃, the pressure of program control type thermocompressor is increased to 800～1300kg/cm
2and be incubated 40～90 minutes, program control type thermocompressor automatic pressure-maintaining between soak; Be incubated follow-up continuation of insurance in 40～90 minutes and press 20 minutes, during temperature be down to 220 ℃; Pressure was down to zero in 10 minutes, and temperature is controlled at 220 ℃, carried out the demoulding until retainer die temperature during lower than 200 ℃.
By adopting technique scheme, the present invention has following beneficial effect:
Described method of the present invention is by being the material of preparing retainer pipe by ether acid anhydride type polyimide molding powder, polypyromelliticimide and heat conduction lubricant, by the material of retainer pipe after drying treatment and proportioning operation on program control type thermocompressor the hot-forming ether acid anhydride type polyimide composite holder pipe that obtains, the ether acid anhydride type polyimide composite holder pipe obtaining is carried out to anneal; The retainer quality of tube blank steel that the present invention produces gently, has effectively improved that Testing Tensile Strength at Elevated Temperature is high, tribological property and thermotolerance.
Embodiment
Below in conjunction with specific embodiment, the invention will be further described, so that those skilled in the art further understands the present invention, but following embodiment is not limiting the scope of the present invention.
The described stable on heating method of raising ether acid anhydride type polyimide retainer pipe, comprises and prepares retainer blank tube material, drying treatment, proportioning operation, hot-forming and anneal, and its concrete operation step is as follows:
(1) prepare retainer blank tube material:
Comprise by weight percentage: 59%～80% ether acid anhydride type polyimide molding powder, 15%～40% polypyromelliticimide and 1%～5% heat conduction lubricant; Described ether acid anhydride type polyimide molding powder, polypyromelliticimide and the particle diameter of heat conduction lubricant be 200 orders; Described heat conduction lubricant is at least comprising any in carbon fiber powder, graphite, carbon nanotube;
(2) drying treatment:
Connect previous step, the retainer blank tube material that previous step is obtained is put into respectively loft drier drying treatment, then crosses respectively 200 mesh sieves independent sealed saving backup; The temperature of described drying treatment is 230 ℃, and be 3h time of drying, and dry rear taking-up is cooled to room temperature;
(3) proportioning operation:
Connect previous step, get respectively by weight percentage dry 60%～80% the ether acid anhydride type polyimide molding powder that obtains in previous step, 15%～40% polypyromelliticimide molding powder and 1%～5% heat conduction lubricant, successively put into machine mixer and stir, make ether acid anhydride type polyimide molding powder matrix material; Stirring number of times in described proportioning operation is 3～5 times, and each time of stirring is controlled at 20～30 seconds, and while stirring, the rotating speed of machine mixer is controlled at 10000～12000 revs/min at every turn;
(4) hot-forming:
Connect previous step, the ether acid anhydride type polyimide molding powder matrix material that previous step is obtained is filled in retainer mould, then retainer mould is placed on program control type thermocompressor, hot-forming ether acid anhydride type polyimide composite holder pipe; At the retainer mould described in hot-forming step, overcoat, fuse, drift and base four parts, consist of, wherein overcoat, fuse and base form retainer die cavity; In retainer mould, the internal diameter size of overcoat is to increase 3mm on the basis of bearing finished products retainer outside dimension, and in retainer mould, the outside dimension of fuse is to dwindle 3mm on the basis of bearing finished products retainer internal diameter size; In retainer mould, the height dimension of overcoat and fuse is on the basis of bearing finished products retainer height dimension, to increase more than 3 times; In retainer mould, the internal diameter size of drift and the outside dimension of fuse match, and the internal diameter size of described base and the outside dimension of fuse match, and the outside dimension of described base and the internal diameter size of overcoat match; The pressure-controlling of described program control type thermocompressor is at 300～600kg/cm
2, suppress the air of getting rid of for 5 minutes in retainer mould, after 5 minutes to retainer mold heated, 60 minutes post-heating to 385 ℃, between heating period, pressure-controlling is at 300～600kg/cm
2; When temperature reaches 385 ℃, the pressure of program control type thermocompressor is increased to 800～1300kg/cm
2and be incubated 40～90 minutes, program control type thermocompressor automatic pressure-maintaining between soak; Be incubated follow-up continuation of insurance in 40～90 minutes and press 20 minutes, during temperature be down to 220 ℃; Pressure was down to zero in 10 minutes, and temperature is controlled at 220 ℃, carried out the demoulding until retainer die temperature during lower than 200 ℃;
(5) anneal:
Connect previous step, the ether acid anhydride type polyimide composite holder pipe that previous step is obtained is placed on sintering in sintering oven, the heat-up rate of sintering oven is controlled at 50～70 ℃/h, while being warming up to 150 ℃ in sintering oven, be incubated 2h, then continue when heat-up rate with 12～20 ℃/h is warming up to 280 ℃ to be incubated 8～10h, the speed with 30～40 ℃/h is cooled to 50 ℃ of taking-ups afterwards.
Embodiment 1
(1) prepare retainer blank tube material:
Components by weight percentage is: 75% ether acid anhydride type polyimide molding powder, 20% polypyromelliticimide and 5% carbon fiber powder;
(2) drying treatment:
The retainer blank tube material that previous step is obtained is put into respectively loft drier drying treatment; The temperature of described drying treatment is 230 ℃, and be 3h time of drying, and dry rear taking-up is cooled to room temperature, then crosses respectively 200 mesh sieves independent sealed saving backup;
(3) proportioning operation:
Get respectively by weight percentage the polypyromelliticimide molding powder of dry 75% the ether acid anhydride type polyimide molding 20% obtaining in previous step and 5% carbon fiber powder, putting into machine mixer stirs 3 times, each time of stirring is controlled at 20 seconds, during each stirring, the rotating speed of machine mixer is controlled at 10000 revs/min, stirring makes ether acid anhydride type polyimide molding powder matrix material, above-mentioned ether acid anhydride type polyimide molding powder is yellow powdery, polypyromelliticimide molding powder is buff powder, carbon fiber is toner shape darkly, through together stirring the ether acid anhydride type polyimide molding powder matrix material obtaining after 3 times, be beige, while using 20 power microscopes to observe ether acid anhydride type polyimide molding powder matrix material, if being beige, color is called without obvious aberration, the ether acid anhydride type polyimide molding powder matrix material of the obvious aberration of nothing is qualified product and sealing saves backup,
(4) hot-forming:
The ether acid anhydride type polyimide molding powder matrix material that previous step is obtained is filled in retainer mould, then retainer mould is placed on program control type thermocompressor, hot-forming ether acid anhydride type polyimide composite holder pipe;
Retainer mould comprises overcoat, fuse, drift and base, and the internal diameter of setting retainer is that d=28.2mm, external diameter are D=35.6mm, highly are H=6.6mm;
In described retainer mould: the internal diameter of described overcoat=described D+3mm=38.6mm, the external diameter of described fuse=described d-3mm=25.2mm, described overcoat height=described fuse height>=3H=19.8mm, the external diameter of described drift and the internal diameter of described overcoat match, the internal diameter of described drift and the external diameter of described fuse match, the internal diameter of described base and the external diameter of described fuse match, and the external diameter of described base and the internal diameter of outer described cover match; The pressure-controlling of program control type thermocompressor is at 500kg/cm
2, the air that the compacting of program control type thermocompressor is got rid of in retainer mould for 5 minutes, implemented heating to retainer mould after 5 minutes, 60 minutes post-heating to 385 ℃, and between heating period, pressure-controlling is at 500kg/cm
2; When temperature reaches 385 ℃, the pressure of program control type thermocompressor is increased to 1000kg/cm
2and be incubated 60 minutes, program control type thermocompressor automatic pressure-maintaining between soak; Be incubated follow-up continuation of insurance in 60 minutes and press 20 minutes, during temperature be down to 220 ℃; Finally, pressure was down to zero in 10 minutes, and temperature is controlled at 220 ℃.Until described retainer die temperature, carry out the demoulding during lower than 200 ℃ and produce ether acid anhydride type polyimide composite holder pipe;
(5) anneal:
The ether acid anhydride type polyimide composite holder pipe that previous step is obtained is placed on sintering in sintering oven, the heat-up rate of sintering oven is controlled at 50 ℃/h, while being warming up to 150 ℃ in sintering oven, be incubated 2h, then continue to be incubated when heat-up rate with 20 ℃/h is warming up to 280 ℃ 8h, with the speed of 40 ℃/h, be cooled to 50 ℃ and take out afterwards.
Ether acid anhydride type polyimide composite holder pipe is to suppress sinter molding under High Temperature High Pressure, and inner remaining larger stress, takes anneal can reduce inner residual mechanical stress, improves the tensile strength of matrix material and the dimensional stability in wide temperature range.
Following table is the performance of the ether acid anhydride type polyimide composite holder pipe of the embodiment of the present invention 1 making
Embodiment 2:
(1) prepare retainer blank tube material:
Components by weight percentage is: 70% ether acid anhydride type polyimide molding powder, 25% polypyromelliticimide and 5% graphite;
(2) drying treatment:
The retainer blank tube material that previous step is obtained is put into respectively loft drier drying treatment; The temperature of described drying treatment is 230 ℃, and be 3h time of drying, and dry rear taking-up is cooled to room temperature, then crosses respectively 200 mesh sieves independent sealed saving backup;
(3) proportioning operation:
Get respectively by weight percentage the polypyromelliticimide molding powder of dry 70% the ether acid anhydride type polyimide molding 25% obtaining in previous step and 5% graphite, putting into machine mixer stirs 3 times, each time of stirring is controlled at 20 seconds, during each stirring, the rotating speed of machine mixer is controlled at 10000 revs/min, stirring makes ether acid anhydride type polyimide molding powder matrix material, above-mentioned ether acid anhydride type polyimide molding powder is yellow powdery, polypyromelliticimide molding powder is buff powder, carbon fiber is toner shape darkly, through together stirring the ether acid anhydride type polyimide molding powder matrix material obtaining after 3 times, be beige, while using 20 power microscopes to observe ether acid anhydride type polyimide molding powder matrix material, if being beige, color is called without obvious aberration, the ether acid anhydride type polyimide molding powder matrix material of the obvious aberration of nothing is qualified product and sealing saves backup,
(4) hot-forming:
The ether acid anhydride type polyimide molding powder matrix material that previous step is obtained is filled in retainer mould, then retainer mould is placed on program control type thermocompressor, hot-forming ether acid anhydride type polyimide composite holder pipe;
Retainer mould comprises overcoat, fuse, drift and base, and the internal diameter of setting retainer is that d=28.2mm, external diameter are D=35.6mm, highly are H=6.6mm;
In described retainer mould: the internal diameter of described overcoat=described D+3mm=38.6mm, the external diameter of described fuse=described d-3mm=25.2mm, described overcoat height=described fuse height>=3H=19.8mm, the external diameter of described drift and the internal diameter of described overcoat match, the internal diameter of described drift and the external diameter of described fuse match, the internal diameter of described base and the external diameter of described fuse match, and the external diameter of described base and the internal diameter of outer described cover match; The pressure-controlling of program control type thermocompressor is at 550kg/cm
2, the air that the compacting of program control type thermocompressor is got rid of in retainer mould for 5 minutes, implemented heating to retainer mould after 5 minutes, 60 minutes post-heating to 385 ℃, and between heating period, pressure-controlling is at 550kg/cm
2; When temperature reaches 385 ℃, the pressure of program control type thermocompressor is increased to 1100kg/cm
2and be incubated 60 minutes, program control type thermocompressor automatic pressure-maintaining between soak; Be incubated follow-up continuation of insurance in 60 minutes and press 20 minutes, during temperature be down to 220 ℃; Finally, pressure was down to zero in 10 minutes, and temperature is controlled at 220 ℃.Until described retainer die temperature, carry out the demoulding during lower than 200 ℃ and produce ether acid anhydride type polyimide composite holder pipe;
(5) anneal:
The ether acid anhydride type polyimide composite holder pipe that previous step is obtained is placed on sintering in sintering oven, the heat-up rate of sintering oven is controlled at 60 ℃/h, while being warming up to 150 ℃ in sintering oven, be incubated 2h, then continue to be incubated when heat-up rate with 15 ℃/h is warming up to 280 ℃ 8h, with the speed of 40 ℃/h, be cooled to 50 ℃ and take out afterwards.
Following table is the performance of the ether acid anhydride type polyimide composite holder pipe of the embodiment of the present invention 2 making
Embodiment 3:
(1) prepare retainer blank tube material:
Components by weight percentage is: 69% ether acid anhydride type polyimide molding powder, 30% polypyromelliticimide and 1% carbon nanotube;
(2) drying treatment:
The retainer blank tube material that previous step is obtained is put into respectively loft drier drying treatment; The temperature of described drying treatment is 230 ℃, and be 3h time of drying, and dry rear taking-up is cooled to room temperature, then crosses respectively 200 mesh sieves independent sealed saving backup;
(3) proportioning operation:
Get respectively by weight percentage the polypyromelliticimide molding powder of dry 69% the ether acid anhydride type polyimide molding 30% obtaining in previous step and 1% carbon nanotube, putting into machine mixer stirs 5 times, each time of stirring is controlled at 30 seconds, during each stirring, the rotating speed of machine mixer is controlled at 12000 revs/min, stirring makes ether acid anhydride type polyimide molding powder matrix material, above-mentioned ether acid anhydride type polyimide molding powder is yellow powdery, polypyromelliticimide molding powder is buff powder, carbon fiber is toner shape darkly, through together stirring the ether acid anhydride type polyimide molding powder matrix material obtaining after 5 times, be beige, while using 20 power microscopes to observe ether acid anhydride type polyimide molding powder matrix material, if being beige, color is called without obvious aberration, the ether acid anhydride type polyimide molding powder matrix material of the obvious aberration of nothing is qualified product and sealing saves backup,
(4) hot-forming:
The ether acid anhydride type polyimide molding powder matrix material that previous step is obtained is filled in retainer mould, then retainer mould is placed on program control type thermocompressor, hot-forming ether acid anhydride type polyimide composite holder pipe;
Retainer mould comprises overcoat, fuse, drift and base, and the internal diameter of setting retainer is that d=28.2mm, external diameter are D=35.6mm, highly are H=6.6mm;
In described retainer mould: the internal diameter of described overcoat=described D+3mm=38.6mm, the external diameter of described fuse=described d-3mm=25.2mm, described overcoat height=described fuse height>=3H=19.8mm, the external diameter of described drift and the internal diameter of described overcoat match, the internal diameter of described drift and the external diameter of described fuse match, the internal diameter of described base and the external diameter of described fuse match, and the external diameter of described base and the internal diameter of outer described cover match; The pressure-controlling of program control type thermocompressor is at 600kg/cm
2, the air that the compacting of program control type thermocompressor is got rid of in retainer mould for 5 minutes, implemented heating to retainer mould after 5 minutes, 60 minutes post-heating to 385 ℃, and between heating period, pressure-controlling is at 600kg/cm
2; When temperature reaches 385 ℃, the pressure of program control type thermocompressor is increased to 1200kg/cm
2and be incubated 60 minutes, program control type thermocompressor automatic pressure-maintaining between soak; Be incubated follow-up continuation of insurance in 60 minutes and press 20 minutes, during temperature be down to 220 ℃; Finally, pressure was down to zero in 10 minutes, and temperature is controlled at 220 ℃.Until described retainer die temperature, carry out the demoulding during lower than 200 ℃ and produce ether acid anhydride type polyimide composite holder pipe;
(5) anneal:
The ether acid anhydride type polyimide composite holder pipe that previous step is obtained is placed on sintering in sintering oven, the heat-up rate of sintering oven is controlled at 50 ℃/h, while being warming up to 150 ℃ in sintering oven, be incubated 2h, then continue to be incubated when heat-up rate with 20 ℃/h is warming up to 280 ℃ 8h, with the speed of 40 ℃/h, be cooled to 50 ℃ and take out afterwards.
Following table is the performance of the ether acid anhydride type polyimide composite holder pipe of the embodiment of the present invention 3 making
By above-mentioned example, can analyze:
1, the ether acid anhydride type polyimide composite holder pipe tensile strength that polypyromelliticimide molding powder modification ether acid anhydride type polyimide makes is higher, and thermotolerance is able to remarkable lifting.
2, the ether acid anhydride type polyimide composite holder pipe that the present invention makes, has that lightweight, tensile strength and hot strength conservation rate are high, a feature such as wear resistance and excellent heat resistance.
3, ether acid anhydride type polyimide composite holder pipe heat-drawn wire (under the pressure of 1.80MPa) is greater than that 280 ℃, 260 ℃ tensile strength conservation rates are not less than 40%, dry friction coefficient is less than 0.20, oil lubrication frictional coefficient is less than 0.05, tensile strength and high temperature conservation rate are high, show that this material can be used for high-temperature bearing field.
Part not in the detailed description of the invention is prior art.
The embodiment selecting in this article in order to disclose goal of the invention of the present invention, currently thinks suitablely, still, will be appreciated that, the present invention is intended to comprise that all belong to all changes and the improvement of the embodiment in this design and invention scope.
Claims (7)
1. improve the stable on heating method of ether acid anhydride type polyimide retainer pipe, comprise and prepare retainer blank tube material, drying treatment, proportioning operation, hot-forming and anneal, it is characterized in that: its concrete operation step is as follows:
(1) prepare retainer blank tube material:
Retainer blank tube material comprises by weight percentage: 59% ~ 80% ether acid anhydride type polyimide molding powder, 15% ~ 40% polypyromelliticimide and 1% ~ 5% heat conduction lubricant;
(2) drying treatment:
Connect previous step, the retainer blank tube material that previous step is obtained is put into respectively loft drier drying treatment, then crosses respectively 200 mesh sieves independent sealed saving backup;
(3) proportioning operation:
Connect previous step, get respectively by weight percentage dry 59% ~ 80% the ether acid anhydride type polyimide molding powder that obtains in previous step, 15% ~ 40% polypyromelliticimide molding powder and 1% ~ 5% heat conduction lubricant, successively put into machine mixer and stir, make ether acid anhydride type polyimide molding powder matrix material;
(4) hot-forming:
Connect previous step, the ether acid anhydride type polyimide molding powder matrix material that previous step is obtained is filled in retainer mould, then retainer mould is placed on program control type thermocompressor, hot-forming ether acid anhydride type polyimide composite holder pipe;
(5) anneal:
Connect previous step, the ether acid anhydride type polyimide composite holder pipe that previous step is obtained is placed on sintering in sintering oven, the heat-up rate of sintering oven is controlled at 50 ~ 70 ℃/h, while being warming up to 150 ℃ in sintering oven, be incubated 2h, then continue when heat-up rate with 12 ~ 20 ℃/h is warming up to 280 ℃ to be incubated 8 ~ 10h, the speed with 30 ~ 40 ℃/h is cooled to 50 ℃ of taking-ups afterwards.
2. the stable on heating method of raising ether acid anhydride type polyimide retainer pipe according to claim 1, is characterized in that: the ether acid anhydride type polyimide molding powder described in step 1, polypyromelliticimide and the particle diameter of heat conduction lubricant be 200 orders.
3. the stable on heating method of raising ether acid anhydride type polyimide retainer pipe according to claim 1, is characterized in that: the heat conduction lubricant described in step 1 is at least comprising any in carbon fiber powder, graphite, carbon nanotube.
4. the stable on heating method of raising ether acid anhydride type polyimide retainer pipe according to claim 1, is characterized in that: the temperature of the drying treatment described in step 2 is 230 ℃, and be 3h time of drying, and dry rear taking-up is cooled to room temperature.
5. the stable on heating method of raising ether acid anhydride type polyimide retainer pipe according to claim 1, it is characterized in that: the stirring number of times in the proportioning operation described in step 3 is 3～5 times, each time of stirring is controlled at 20～30 seconds, and while stirring, the rotating speed of machine mixer is controlled at 10000～12000 revs/min at every turn.
6. the stable on heating method of raising ether acid anhydride type polyimide retainer pipe according to claim 1, at the retainer mould described in hot-forming step, overcoat, fuse, drift and base four parts, consist of, wherein overcoat, fuse and base form retainer die cavity; In retainer mould, the internal diameter size of overcoat is to increase 3mm on the basis of bearing finished products retainer outside dimension, and in retainer mould, the outside dimension of fuse is to dwindle 3mm on the basis of bearing finished products retainer internal diameter size; In retainer mould, the height dimension of overcoat and fuse is on the basis of bearing finished products retainer height dimension, to increase more than 3 times; In retainer mould, the internal diameter size of drift and the outside dimension of fuse match, and the internal diameter size of described base and the outside dimension of fuse match, and the outside dimension of described base and the internal diameter size of overcoat match.
7. the stable on heating method of raising ether acid anhydride type polyimide retainer pipe according to claim 1, in the pressure-controlling of the program control type thermocompressor described in hot-forming step at 300 ~ 600kg/cm
2, suppress the air of getting rid of for 5 minutes in retainer mould, after 5 minutes to retainer mold heated, 60 minutes post-heating to 385 ℃, between heating period, pressure-controlling is at 300 ~ 600kg/cm
2; When temperature reaches 385 ℃, the pressure of program control type thermocompressor is increased to 800 ~ 1300 kg/cm
2and be incubated 40 ~ 90 minutes, program control type thermocompressor automatic pressure-maintaining between soak; Be incubated follow-up continuation of insurance in 40 ~ 90 minutes and press 20 minutes, during temperature be down to 220 ℃; Pressure was down to zero in 10 minutes, and temperature is controlled at 220 ℃, carried out the demoulding until retainer die temperature during lower than 200 ℃.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310683681.1A CN103756313B (en) | 2013-12-13 | 2013-12-13 | Method used for increasing hear resistance of ketone-anhydride type polyimide retainer tube blank |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310683681.1A CN103756313B (en) | 2013-12-13 | 2013-12-13 | Method used for increasing hear resistance of ketone-anhydride type polyimide retainer tube blank |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN103756313A true CN103756313A (en) | 2014-04-30 |
| CN103756313B CN103756313B (en) | 2017-01-11 |
Family
ID=50523649
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201310683681.1A Active CN103756313B (en) | 2013-12-13 | 2013-12-13 | Method used for increasing hear resistance of ketone-anhydride type polyimide retainer tube blank |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN103756313B (en) |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2017113180A1 (en) * | 2015-12-30 | 2017-07-06 | Jf Polymers (Suzhou) Co. Ltd. | Methods and systems for improving the heat resistance of 3d-printed objects |
| CN109808114A (en) * | 2018-12-29 | 2019-05-28 | 洛阳轴承研究所有限公司 | A kind of bearing holder material and preparation method thereof, bearing retainer and preparation method thereof |
| CN110016229A (en) * | 2018-01-09 | 2019-07-16 | 洛阳轴承研究所有限公司 | Low fuel-displaced rate micropore core valve material of one kind and preparation method thereof |
| CN110028788A (en) * | 2018-01-11 | 2019-07-19 | 洛阳轴承研究所有限公司 | A kind of composite polyimide material, porous polyimide retainer and preparation method thereof, bearing |
| CN113147105A (en) * | 2021-04-23 | 2021-07-23 | 中国科学院兰州化学物理研究所 | Porous polyimide oil storage and retention structure and preparation method and application thereof |
Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH0364355A (en) * | 1989-08-02 | 1991-03-19 | Shin Etsu Chem Co Ltd | Composition for protection of semiconductor element |
| JPH1077406A (en) * | 1996-07-29 | 1998-03-24 | E I Du Pont De Nemours & Co | Antistatic aromatic polyimide film |
| JP2001179911A (en) * | 1999-12-27 | 2001-07-03 | Ube Ind Ltd | Heat-resistant resin board and method of manufacturing the same |
| CN101629601A (en) * | 2009-08-04 | 2010-01-20 | 重庆斯凯迪轴瓦有限公司 | High molecular abrasion-proof bearing bush |
| CN103160124A (en) * | 2013-02-26 | 2013-06-19 | 洛阳轴研科技股份有限公司 | Method for producing holder blank with ether anhydride type polyimide molding powder composite material |
| CN103232706A (en) * | 2013-05-09 | 2013-08-07 | 蔡德扬 | High-temperature-resistant modified polyimide and preparation method thereof |
| CN103305001A (en) * | 2013-05-15 | 2013-09-18 | 洛阳轴研科技股份有限公司 | Manufacturing method of ketone-anhydride type polyimide composite retainer tube blank |
-
2013
- 2013-12-13 CN CN201310683681.1A patent/CN103756313B/en active Active
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH0364355A (en) * | 1989-08-02 | 1991-03-19 | Shin Etsu Chem Co Ltd | Composition for protection of semiconductor element |
| JPH1077406A (en) * | 1996-07-29 | 1998-03-24 | E I Du Pont De Nemours & Co | Antistatic aromatic polyimide film |
| JP2001179911A (en) * | 1999-12-27 | 2001-07-03 | Ube Ind Ltd | Heat-resistant resin board and method of manufacturing the same |
| CN101629601A (en) * | 2009-08-04 | 2010-01-20 | 重庆斯凯迪轴瓦有限公司 | High molecular abrasion-proof bearing bush |
| CN103160124A (en) * | 2013-02-26 | 2013-06-19 | 洛阳轴研科技股份有限公司 | Method for producing holder blank with ether anhydride type polyimide molding powder composite material |
| CN103232706A (en) * | 2013-05-09 | 2013-08-07 | 蔡德扬 | High-temperature-resistant modified polyimide and preparation method thereof |
| CN103305001A (en) * | 2013-05-15 | 2013-09-18 | 洛阳轴研科技股份有限公司 | Manufacturing method of ketone-anhydride type polyimide composite retainer tube blank |
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2017113180A1 (en) * | 2015-12-30 | 2017-07-06 | Jf Polymers (Suzhou) Co. Ltd. | Methods and systems for improving the heat resistance of 3d-printed objects |
| CN110016229A (en) * | 2018-01-09 | 2019-07-16 | 洛阳轴承研究所有限公司 | Low fuel-displaced rate micropore core valve material of one kind and preparation method thereof |
| CN110016229B (en) * | 2018-01-09 | 2021-06-01 | 洛阳轴承研究所有限公司 | Low-oil-outlet-rate microporous core valve material and preparation method thereof |
| CN110028788A (en) * | 2018-01-11 | 2019-07-19 | 洛阳轴承研究所有限公司 | A kind of composite polyimide material, porous polyimide retainer and preparation method thereof, bearing |
| CN109808114A (en) * | 2018-12-29 | 2019-05-28 | 洛阳轴承研究所有限公司 | A kind of bearing holder material and preparation method thereof, bearing retainer and preparation method thereof |
| CN109808114B (en) * | 2018-12-29 | 2021-03-09 | 洛阳轴承研究所有限公司 | Preparation method of bearing retainer material and preparation method of bearing retainer |
| CN113147105A (en) * | 2021-04-23 | 2021-07-23 | 中国科学院兰州化学物理研究所 | Porous polyimide oil storage and retention structure and preparation method and application thereof |
Also Published As
| Publication number | Publication date |
|---|---|
| CN103756313B (en) | 2017-01-11 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN103756313A (en) | Method used for increasing hear resistance of ketone-anhydride type polyimide retainer tube blank | |
| CN104707931B (en) | A kind of manufacture method of large-sized high-temperature alloy dish class forging part | |
| CN103160124B (en) | Method for producing holder blank with ether anhydride type polyimide molding powder composite material | |
| CN102000825A (en) | Method for manufacturing driving gear of motorcycle clutch | |
| CN100448328C (en) | Production method of ultrohigh power graphite electrode | |
| CN102951634A (en) | Oversized isostatic pressing graphite and production method thereof | |
| CN102962455A (en) | Powder metallurgy injection molding process | |
| CN104493167A (en) | Method for forming powder high-temperature alloy annular member | |
| CN102407337A (en) | Method for manufacturing titanium and titanium alloy powder metallurgy special-shaped pieces | |
| CN103252491B (en) | Method for preparing powder metallurgy of engine piston pin | |
| CN102773482B (en) | Method for manufacturing butterfly valve rod by powder metallurgy | |
| CN108083803A (en) | A kind of preparation method and graphite product of mold compression moulding graphite product | |
| CN103182761B (en) | Method for manufacturing retainer pipe blank with fusible polyimide molding powder as base material | |
| CN204867261U (en) | Large -scale axle journal class forging forges mould | |
| CN101564809A (en) | Preparation method of covered metal spare parts | |
| CN103305001B (en) | A kind of making method of ketone acid anhydride type polyimide composite holder pipe | |
| CN103706741B (en) | Hot forging and molding process for oxygen free copper material | |
| CN103357865B (en) | A kind of enhancing mixes titanium powder metallurgical material and preparation method thereof | |
| CN105689708B (en) | A kind of HS311 base steels copper moulds the production technology of self-lubricating material | |
| CN104046024A (en) | Preparation method of tubular polyimide composite material for bearing retainers | |
| CN103771404B (en) | A kind of preparation method of oilless bearing graphite rod | |
| CN102773487A (en) | Powder metallurgy preparation method of check valve clack | |
| CN102773484A (en) | Method for manufacturing ball-shaped check valve body by powder metallurgy | |
| CN103613905A (en) | Glass fiber-reinforced polyether-ether-ketone fracturing ball for oil exploration and manufacturing method for fracturing ball | |
| CN102773485B (en) | Method for manufacturing check valve core by powder metallurgy |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant | ||
| TR01 | Transfer of patent right | ||
| TR01 | Transfer of patent right |
Effective date of registration: 20180511 Address after: 471000 No. 1 axis research road, Jianxi science and Technology Industrial Park, Luoyang, Henan Patentee after: Luoyang Bearing Research Institute Address before: 471039 Fenghua Road 6, hi tech Development Zone, Luoyang, Henan. Patentee before: Zhouyan Science and Technology Co., Ltd., Luoyang |