CN1730262A - Compression molding technique for thermostable polyimide and its composite material - Google Patents
Compression molding technique for thermostable polyimide and its composite material Download PDFInfo
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- CN1730262A CN1730262A CN 200510046677 CN200510046677A CN1730262A CN 1730262 A CN1730262 A CN 1730262A CN 200510046677 CN200510046677 CN 200510046677 CN 200510046677 A CN200510046677 A CN 200510046677A CN 1730262 A CN1730262 A CN 1730262A
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- polyimide
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Abstract
The invention relates to the processing technique art of the polyimide composite material. It is characterized in that it follows such steps: first the application temperature range of the aromatic polyimide material higher than 300 Deg.C; selecting filling agent provided with strengthening dynamic property, enhancing heatproof and lubricating; wet blending or infiltrating uniformly the polyimide material and filling agent or unidirectional fiber and fabric and drying them to the constant weight, to make polyimide special powder and prepreg; after pressurization and insulation said powder or prepreg compression moulding, with setting pressure 5-70MPa, temperature `50-550 Deg.C, and timing 10 minutes to 4 hours; trapezoid heating it to the allowed maximum temperature of said element, after shape procession for 1-80 hours to get the element end product or slug of the polyimide composite material. The purpose of the invention is to dissolve the problem by applying to section bar machining method for polyimide material, such as intractability, low yield, high fabrication cost.
Description
Technical field:
The invention belongs to the field of aromatic polyimide and composite material moulded moulding process thereof, particularly relate to a kind of research of adopting graphite and carbon fiber to strengthen the die press technology for forming of composite polyimide material.
Background technology:
Polyimides is the very superior heat-proof macromolecule material of a kind of performance, be referred to as " Problemsoolver " (expert who puts the axe in the helve) abroad, has outstanding properties not only at structural material (as special engineering plastics, advanced composite material), insulating materials (as book film, enamel-covered wire), and at functional material aspects such as (as thermostable transparent material, low-k radiation hardness).The general extensive use high-tech sector of this material gets most of the attention owing to having preeminent performance for a long time.
Existing its technology of a lot of products of China is that introduction is external.It is to adopt polyimide material that part is arranged in former design, but just adopts material itself, and the polyimide material of domestic production is sheet material and bar, adopting the method stock utilization of machining is 30%, and yield rate only is 5%, and design of part intensity is low, and is easily broken.Especially surpass 300 ℃ of fire resistant polyimide materials because its difficulty of processing is higher, material price is more expensive again.For this reason, if can adopt the technology of compression molding to manufacture a product, the quality that can improve product can reduce production costs again.
Summary of the invention:
The invention provides a kind of process of the compression molding to fire resistant polyimide and composite thereof, its purpose is to solve the problem that adopts aspects such as section bar difficulty of processing that machining process causes yield rate higher, product is low, product quality does not reach specification requirement, production cost height existence at polyimide material.
The present invention is achieved through the following technical solutions:
The process of the compression molding of fire resistant polyimide and composite thereof is characterized in that processing step carries out as follows:
A, according to serviceability temperature aromatic polyimide material more than 300 ℃;
B, select to have strengthen mechanical property, improve heatproof, dielectric properties and the material that improves self-lubricating property be as inserts;
C, will screen the aromatic polyimide material that obtains and inserts or unidirectional fibre and braid and adopt wet method to carry out batch mixing or infiltration, dry to constant weight after evenly, and make uniform polyimides special use powder or give and soak material;
D, this powder or give soak material in mould through the pressure heat-preserving compression molding, pressure limit is at 5～70MPa, temperature is in 150～550 ℃ of scopes, the time is 10 minutes to 4 hours;
E, the trapezoidal required maximum temperature of this part that is warmed up to of employing are handled through 1～80 hour typing, and what typing obtained after handling is the parts finished product or the blank of composite polyimide material;
Described have the material that strengthens mechanical property, improve heatproof and improve self-lubricating property as inserts, this material is generally fortifying fibre class material, graphite fibre, carbon fiber, glass fibre, aramid fiber, superhigh molecular weight polyethylene fibers, boron fibre, whisker and nano material; The material that improves heatproof and dielectric properties adopts graphite, rare earth material; Improve material graphite, curing aluminium, the fluorinated material of self-lubricating property, inserts accounts for 0.005～70% of polyimides weight;
Described wet method is a polyimides at polymerization state or the state not before the desolventizing time.
To the requirement of mould is alternating temperature between the normal temperature to 600 ℃, and the expansion rate of mould is less than 1.1;
Adopt moulding press to handle in pressure heat-preserving, typing handling procedure, moulding press adopts the electric heating hydraulic way, and temperature range is in 0～600 ℃.
Advantage of the present invention and effect:
Adopt the process of fire resistant polyimide of the present invention and composite material moulded moulding thereof, the yield rate of product is 100%, product processed doubles than section bar machining through the experiment structural behaviour, every technical indicators such as the mechanical property of polyimide parts, physical dimension all are better than adopting the index of the resulting product of machining process of bar turning production polyimide parts, simultaneously, production cost also only is to adopt 40% of machining process production cost originally, has satisfied client's instructions for use.
Description of drawings:
Accompanying drawing 1 is a process chart of the present invention.
The specific embodiment:
At serviceability temperature more than 300 ℃ the fire resistant polyimide material carry out test step by step, determine the matrix resin and the inserts of polyimides.(TMA), heat decomposition temperature determines to adopt the PGAT of U.S. PE company to carry out thermogravimetric analysis (TGA), and we think also can illustrate the product thermal stability that adopts this processes by These parameters.
Determining of resin formula; Selection has TGA and TMA analyzes, and has selected 3 matrix resins as the basis in 5 prescriptions.
Selecting of inserts; Selection have strengthen mechanical property, improve heatproof, dielectric properties and the material that improves self-lubricating property be as inserts; Described have the material that strengthens mechanical property, improve heatproof and improve self-lubricating property as inserts, this material is generally fortifying fibre class material, graphite fibre, carbon fiber, glass fibre, aramid fiber, superhigh molecular weight polyethylene fibers, boron fibre, whisker and nano material; The material that improves heatproof and dielectric properties adopts graphite, rare earth material; Improve material graphite, curing aluminium, the fluorinated material of self-lubricating property, according to The performance test results, in the polyimide resin material of selecting for use, determine with a kind of more than graphite, the carbon fiber etc. or several be inserts, its consumption uses the position to determine that inserts accounts for 0.005～70% of polyimides weight according to parts.The weight 5～30% of the shared polyimides of inserts of strengthening the property for raising, the weight that improves the shared polyimides of inserts of dielectric properties is 0.005～5%, the weight that improves the shared polyimides of inserts of heatproof is 5～40%, improves the weight 5～70% of the shared polyimides of inserts of self-lubricating property.
The preparation method determines; We find that in Research on processing technology experiment the dry method batch mixing easily produces static, for obtaining good interface, adopt material by wet type mixing or infiltration, finally make thin and special-purpose powder fire resistant polyimide uniformly or give and soak material.
So-called wet method is the state of polyimides under polymerization state or not before the desolventizing time.
Determining of mould: mould is that metal material is made, and annealing before its processing is quenched after the processing and carburization process, finish grindes then.To the requirement of mould be high temperature resistant, distortion is little, alternating temperature that can anti-normal temperature to 600 ℃, expansion rate is less than 1.1.
Determining of tonnage and temperature-time: choose 5 force value of setting according to the characteristics of PP Pipe Compound, with constant temperature, regularly, select an optimum pressure value.Under level pressure power, the situation of fixing time, determine 5 adjacent temperature, select the processing temperature an of the best again.Under the fixing situation of pressure and temperature, select 5 different process times, select the short process time that can ensure the quality of products again of the production time.General pressure limit is at 5～70MPa, and temperature is in 150～550 ℃ of scopes, and the time is value in 10 minutes to 4 hours.
Polyimides PP Pipe Compound or give the preparation of soaking material; Need constant temperature to constant weight, weigh and the external form cutting according to the weight sub-material of parts then.
The preparation of former; Adopt moulding press to handle in pressure heat-preserving, typing handling procedure, moulding press adopts the electric heating hydraulic way, and temperature range is in 0～600 ℃.With the moulding press preheating, check whether instrument is accurate.
The preparation of mould, the check die size is placed on preheating on the moulding press before using.
With dividing good PP Pipe Compound or giving soaking and expect to insert in the mould, be placed on the moulding press.Configuring temperature, pressure and time processes, and process is guarded by the special messenger.
Accompanying drawing 1 is a process chart of the present invention; Adopt the trapezoidal required maximum temperature of this part that is warmed up in the typing handling procedure wherein, through 1～80h.
Following table is that the parts of compression molding advanced High Temperature Resistant Polyimide Composites and section bar machine add the contrast that every performance of producing the polyimides parts is done;
Sequence number project section bar machine adds 1 section bar machine and adds 2 section bar machines and add 3
Compression molding
23 ℃ 134 107 118 of 1 compression strength
164
MPa 250℃ 79.1 71.7 70.8
102
23 ℃ 68.2 54.7 61.4 of 2 hot strength
72.6
MPa 250℃ 54.7 34.6 35.2
58.5
23 ℃ 112 95 97.8 of 3 bending strength
123.7
MPa 250℃ 65.8 5.3 49.4
78.9
4 impact strengths 18.8 11.3 13.7
16.7
23 ℃ 5.3 4.2 3.2 of 5 stretch percentage elongation
7.6
％ 250℃ 4.2 2.2 3.98
8.9
6 relative densities 1.50 1.55 1.51
1.38
400 ℃ 1.7 3.9 4.1 of 7 hot property
1.51
Following deformation %
8 average line expansion series coefficients 4.3 9.8 10.3
4.0
×10
-5℃
9 hot Td 536.9 496.4 536.7
550.8
Lose T5% 500.6 444.1 507.4
465.5
Heavy T10% 529.6 509.5 529.1
542.7
℃
Claims (5)
1, the process of the compression molding of fire resistant polyimide and composite thereof is characterized in that processing step carries out as follows:
A, according to serviceability temperature aromatic polyimide material more than 300 ℃;
B, select to have strengthen mechanical property, improve heatproof, dielectric properties and the material that improves self-lubricating property be as inserts;
C, will screen the aromatic polyimide material that obtains and inserts or unidirectional fibre and braid and adopt wet method to carry out batch mixing or infiltration, dry to constant weight after evenly, and make uniform polyimides special use powder or give and soak material;
D, this powder or give soak material in mould through the pressure heat-preserving compression molding, pressure limit is at 5～70MPa, temperature is in 150～550 ℃ of scopes, the time is 10 minutes to 4 hours;
E, the trapezoidal required maximum temperature of this part that is warmed up to of employing are handled through 1～80 hour typing, and what typing obtained after handling is the parts finished product or the blank of composite polyimide material;
2, the process of the compression molding of a kind of advanced High Temperature Resistant Polyimide Composites according to claim 1, it is characterized in that: described have the material that strengthens mechanical property, improve heatproof and improve self-lubricating property as inserts, this material is generally fortifying fibre class material, graphite fibre, carbon fiber, glass fibre, aramid fiber, superhigh molecular weight polyethylene fibers, boron fibre, whisker and nano material; The material that improves heatproof and dielectric properties adopts graphite, rare earth material; Improve material graphite, curing aluminium, the fluorinated material of self-lubricating property, inserts accounts for 0.005～70% of polyimides weight;
3, the process of the compression molding of a kind of advanced High Temperature Resistant Polyimide Composites according to claim 1 is characterized in that: the wet method described in the claim 1 is a polyimides at polymerization state or the state not before the desolventizing time;
4, the process of the compression molding of a kind of advanced High Temperature Resistant Polyimide Composites according to claim 1 is characterized in that: be alternating temperature between the normal temperature to 600 ℃ to the requirement of mould in the claim 1, the expansion rate of mould is less than 1.1;
5, the process of the compression molding of a kind of advanced High Temperature Resistant Polyimide Composites according to claim 1, it is characterized in that: in pressure heat-preserving, typing handling procedure, adopt moulding press to handle, moulding press adopts the electric heating hydraulic way, and temperature range is between 0～600 ℃.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200510046677 CN1730262A (en) | 2005-06-15 | 2005-06-15 | Compression molding technique for thermostable polyimide and its composite material |
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| CN 200510046677 CN1730262A (en) | 2005-06-15 | 2005-06-15 | Compression molding technique for thermostable polyimide and its composite material |
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| CN1730262A true CN1730262A (en) | 2006-02-08 |
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| CN 200510046677 Pending CN1730262A (en) | 2005-06-15 | 2005-06-15 | Compression molding technique for thermostable polyimide and its composite material |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101787208A (en) * | 2010-03-31 | 2010-07-28 | 上海交通大学 | Method for preparing rare-earth modified polyethylene fiber polyimide composite materials |
| CN102275311A (en) * | 2011-07-12 | 2011-12-14 | 北京化工大学 | Reaction molding method for polyimide composites |
| CN102863781A (en) * | 2012-09-25 | 2013-01-09 | 浙江吉利汽车研究院有限公司杭州分公司 | Fiber resin engine gasket and preparation method thereof |
| CN104312190A (en) * | 2014-10-14 | 2015-01-28 | 荣成复合材料有限公司 | Composite material for lift pedals and cages |
| CN104962167A (en) * | 2015-06-18 | 2015-10-07 | 湖州湖杰漆业有限公司 | High-temperature-resistant insulating paint and preparation method thereof |
| CN107760001A (en) * | 2016-06-15 | 2018-03-06 | 朱森 | A kind of impact resistance anti-block sewer lid high polymer material |
| CN113696514A (en) * | 2021-08-17 | 2021-11-26 | 江苏泰氟隆科技有限公司 | Manufacturing process of glass fiber reinforced polyimide gasket |
-
2005
- 2005-06-15 CN CN 200510046677 patent/CN1730262A/en active Pending
Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101787208A (en) * | 2010-03-31 | 2010-07-28 | 上海交通大学 | Method for preparing rare-earth modified polyethylene fiber polyimide composite materials |
| CN102275311A (en) * | 2011-07-12 | 2011-12-14 | 北京化工大学 | Reaction molding method for polyimide composites |
| CN102275311B (en) * | 2011-07-12 | 2013-04-17 | 北京化工大学 | Reaction molding method for polyimide composites |
| CN102863781A (en) * | 2012-09-25 | 2013-01-09 | 浙江吉利汽车研究院有限公司杭州分公司 | Fiber resin engine gasket and preparation method thereof |
| CN104312190A (en) * | 2014-10-14 | 2015-01-28 | 荣成复合材料有限公司 | Composite material for lift pedals and cages |
| CN104962167A (en) * | 2015-06-18 | 2015-10-07 | 湖州湖杰漆业有限公司 | High-temperature-resistant insulating paint and preparation method thereof |
| CN107760001A (en) * | 2016-06-15 | 2018-03-06 | 朱森 | A kind of impact resistance anti-block sewer lid high polymer material |
| CN107760000A (en) * | 2016-06-15 | 2018-03-06 | 朱森 | A kind of preparation method of impact resistance anti-block sewer lid high polymer material |
| CN113696514A (en) * | 2021-08-17 | 2021-11-26 | 江苏泰氟隆科技有限公司 | Manufacturing process of glass fiber reinforced polyimide gasket |
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