CN1593908A - Heat resistant polyimide film composite casing pipe, preparation method and equipment thereof - Google Patents
Heat resistant polyimide film composite casing pipe, preparation method and equipment thereof Download PDFInfo
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- CN1593908A CN1593908A CN 200410024495 CN200410024495A CN1593908A CN 1593908 A CN1593908 A CN 1593908A CN 200410024495 CN200410024495 CN 200410024495 CN 200410024495 A CN200410024495 A CN 200410024495A CN 1593908 A CN1593908 A CN 1593908A
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- polyamic acid
- acid resin
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- 238000002360 preparation method Methods 0.000 title claims abstract description 12
- 239000002131 composite material Substances 0.000 title claims description 39
- 229920001646 UPILEX Polymers 0.000 title 1
- 239000011347 resin Substances 0.000 claims abstract description 27
- 229920005989 resin Polymers 0.000 claims abstract description 27
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 claims description 24
- 238000001035 drying Methods 0.000 claims description 24
- 229920005575 poly(amic acid) Polymers 0.000 claims description 24
- 238000004026 adhesive bonding Methods 0.000 claims description 23
- 239000007921 spray Substances 0.000 claims description 22
- 239000010409 thin film Substances 0.000 claims description 19
- 229920001721 polyimide Polymers 0.000 claims description 18
- 239000004642 Polyimide Substances 0.000 claims description 17
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 15
- 239000010439 graphite Substances 0.000 claims description 15
- 229910002804 graphite Inorganic materials 0.000 claims description 15
- HFACYLZERDEVSX-UHFFFAOYSA-N benzidine Chemical compound C1=CC(N)=CC=C1C1=CC=C(N)C=C1 HFACYLZERDEVSX-UHFFFAOYSA-N 0.000 claims description 14
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims description 13
- 238000005245 sintering Methods 0.000 claims description 12
- 229910001882 dioxygen Inorganic materials 0.000 claims description 11
- 150000001412 amines Chemical class 0.000 claims description 10
- HLBLWEWZXPIGSM-UHFFFAOYSA-N 4-Aminophenyl ether Chemical compound C1=CC(N)=CC=C1OC1=CC=C(N)C=C1 HLBLWEWZXPIGSM-UHFFFAOYSA-N 0.000 claims description 9
- GTDPSWPPOUPBNX-UHFFFAOYSA-N ac1mqpva Chemical compound CC12C(=O)OC(=O)C1(C)C1(C)C2(C)C(=O)OC1=O GTDPSWPPOUPBNX-UHFFFAOYSA-N 0.000 claims description 9
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 8
- WFKAJVHLWXSISD-UHFFFAOYSA-N isobutyramide Chemical compound CC(C)C(N)=O WFKAJVHLWXSISD-UHFFFAOYSA-N 0.000 claims description 8
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 7
- 229910052782 aluminium Inorganic materials 0.000 claims description 7
- 238000000576 coating method Methods 0.000 claims description 7
- -1 imvite Chemical compound 0.000 claims description 7
- 229920003223 poly(pyromellitimide-1,4-diphenyl ether) Polymers 0.000 claims description 7
- 239000011248 coating agent Substances 0.000 claims description 6
- 239000011256 inorganic filler Substances 0.000 claims description 6
- 229910003475 inorganic filler Inorganic materials 0.000 claims description 6
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 claims description 6
- 229910052582 BN Inorganic materials 0.000 claims description 5
- PZNSFCLAULLKQX-UHFFFAOYSA-N Boron nitride Chemical compound N#B PZNSFCLAULLKQX-UHFFFAOYSA-N 0.000 claims description 5
- 229910000604 Ferrochrome Inorganic materials 0.000 claims description 5
- 150000004984 aromatic diamines Chemical class 0.000 claims description 5
- 125000003118 aryl group Chemical group 0.000 claims description 5
- ANSXAPJVJOKRDJ-UHFFFAOYSA-N furo[3,4-f][2]benzofuran-1,3,5,7-tetrone Chemical compound C1=C2C(=O)OC(=O)C2=CC2=C1C(=O)OC2=O ANSXAPJVJOKRDJ-UHFFFAOYSA-N 0.000 claims description 5
- 239000000203 mixture Substances 0.000 claims description 5
- 239000010935 stainless steel Substances 0.000 claims description 5
- 229910001220 stainless steel Inorganic materials 0.000 claims description 5
- 239000002313 adhesive film Substances 0.000 claims description 4
- FPAFDBFIGPHWGO-UHFFFAOYSA-N dioxosilane;oxomagnesium;hydrate Chemical compound O.[Mg]=O.[Mg]=O.[Mg]=O.O=[Si]=O.O=[Si]=O.O=[Si]=O.O=[Si]=O FPAFDBFIGPHWGO-UHFFFAOYSA-N 0.000 claims description 4
- 239000010408 film Substances 0.000 claims description 4
- 239000000377 silicon dioxide Substances 0.000 claims description 4
- 239000002904 solvent Substances 0.000 claims description 4
- BBTGUNMUUYNPLH-UHFFFAOYSA-N 5-[4-[(1,3-dioxo-2-benzofuran-5-yl)oxy]phenoxy]-2-benzofuran-1,3-dione Chemical compound C1=C2C(=O)OC(=O)C2=CC(OC2=CC=C(C=C2)OC=2C=C3C(=O)OC(C3=CC=2)=O)=C1 BBTGUNMUUYNPLH-UHFFFAOYSA-N 0.000 claims description 3
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 claims description 3
- 238000001816 cooling Methods 0.000 claims description 3
- 229910052750 molybdenum Inorganic materials 0.000 claims description 3
- 239000011733 molybdenum Substances 0.000 claims description 3
- MYMOFIZGZYHOMD-UHFFFAOYSA-N Dioxygen Chemical compound O=O MYMOFIZGZYHOMD-UHFFFAOYSA-N 0.000 claims description 2
- 240000007594 Oryza sativa Species 0.000 claims description 2
- 235000007164 Oryza sativa Nutrition 0.000 claims description 2
- 238000002156 mixing Methods 0.000 claims description 2
- 239000002245 particle Substances 0.000 claims description 2
- 238000006116 polymerization reaction Methods 0.000 claims description 2
- 239000002243 precursor Substances 0.000 claims description 2
- 235000009566 rice Nutrition 0.000 claims description 2
- 238000005303 weighing Methods 0.000 claims 1
- 238000000034 method Methods 0.000 abstract description 25
- 238000004519 manufacturing process Methods 0.000 abstract description 16
- 239000012528 membrane Substances 0.000 abstract description 7
- 238000010438 heat treatment Methods 0.000 abstract description 2
- 239000010410 layer Substances 0.000 abstract 5
- 239000004952 Polyamide Substances 0.000 abstract 2
- 229920002647 polyamide Polymers 0.000 abstract 2
- 229920006122 polyamide resin Polymers 0.000 abstract 2
- KRHYYFGTRYWZRS-UHFFFAOYSA-M Fluoride anion Chemical compound [F-] KRHYYFGTRYWZRS-UHFFFAOYSA-M 0.000 abstract 1
- 238000005452 bending Methods 0.000 abstract 1
- 239000011247 coating layer Substances 0.000 abstract 1
- 150000001875 compounds Chemical class 0.000 abstract 1
- 238000010924 continuous production Methods 0.000 abstract 1
- 238000009776 industrial production Methods 0.000 abstract 1
- 238000007790 scraping Methods 0.000 abstract 1
- CYIDZMCFTVVTJO-UHFFFAOYSA-N pyromellitic acid Chemical compound OC(=O)C1=CC(C(O)=O)=C(C(O)=O)C=C1C(O)=O CYIDZMCFTVVTJO-UHFFFAOYSA-N 0.000 description 18
- 239000000463 material Substances 0.000 description 11
- 210000002469 basement membrane Anatomy 0.000 description 10
- 239000006229 carbon black Substances 0.000 description 9
- 235000019241 carbon black Nutrition 0.000 description 9
- 239000000839 emulsion Substances 0.000 description 9
- 239000007787 solid Substances 0.000 description 9
- 229920001343 polytetrafluoroethylene Polymers 0.000 description 8
- 239000004810 polytetrafluoroethylene Substances 0.000 description 8
- CBCKQZAAMUWICA-UHFFFAOYSA-N 1,4-phenylenediamine Chemical compound NC1=CC=C(N)C=C1 CBCKQZAAMUWICA-UHFFFAOYSA-N 0.000 description 6
- ZUOUZKKEUPVFJK-UHFFFAOYSA-N diphenyl Chemical compound C1=CC=CC=C1C1=CC=CC=C1 ZUOUZKKEUPVFJK-UHFFFAOYSA-N 0.000 description 4
- 210000004379 membrane Anatomy 0.000 description 3
- 239000004305 biphenyl Substances 0.000 description 2
- 235000010290 biphenyl Nutrition 0.000 description 2
- 229920001577 copolymer Polymers 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 239000003292 glue Substances 0.000 description 2
- 238000005507 spraying Methods 0.000 description 2
- TVEXGJYMHHTVKP-UHFFFAOYSA-N 6-oxabicyclo[3.2.1]oct-3-en-7-one Chemical compound C1C2C(=O)OC1C=CC2 TVEXGJYMHHTVKP-UHFFFAOYSA-N 0.000 description 1
- 229910000838 Al alloy Inorganic materials 0.000 description 1
- SECXISVLQFMRJM-UHFFFAOYSA-N N-Methylpyrrolidone Chemical class CN1CCCC1=O SECXISVLQFMRJM-UHFFFAOYSA-N 0.000 description 1
- 239000000853 adhesive Substances 0.000 description 1
- 230000001070 adhesive effect Effects 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 150000002170 ethers Chemical class 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 239000000835 fiber Substances 0.000 description 1
- 239000000945 filler Substances 0.000 description 1
- 239000006260 foam Substances 0.000 description 1
- 235000013305 food Nutrition 0.000 description 1
- 238000001802 infusion Methods 0.000 description 1
- KQNPFQTWMSNSAP-UHFFFAOYSA-N isobutyric acid Chemical compound CC(C)C(O)=O KQNPFQTWMSNSAP-UHFFFAOYSA-N 0.000 description 1
- 239000003973 paint Substances 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 229920003023 plastic Polymers 0.000 description 1
- 239000009719 polyimide resin Substances 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- 238000003892 spreading Methods 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
Landscapes
- Laminated Bodies (AREA)
- Manufacture Of Macromolecular Shaped Articles (AREA)
Abstract
The invention relates to a kind of polyamide compound annular membrane tubes that can bear heating and the preparative method and production equipments that can form the ability of continuous production. It can use on duplicator, Fax-machine and scanner. The annular membrane tubes are composed of membrane coating layer, conducting layer and fluoride resin layer. The preparing methods are as following: (1) daubing the tubes, whose plane is as bright as mirror, with polyamide resin and then make curing, (2) daubing the inner layer of the polyamide membrane with conducting layer, (3) daubing the conducting layer with polyamide resin. This machine comprise two locating mould and one scraping mould. This invention has the good qualities such as good tenacity, high ability of bending and stretching, long-lived use. It also has the advantage of continuous industrial production.
Description
Technical field
The present invention relates to a kind of heat resisting polyimides amine thin film composite sleeve, and can form the preparation method and the production equipment of the production capacity of serialization.
Background technology
Because polyimides has outstanding advantage aspect combination property, be widely used in civilian industries such as military fields such as Aeronautics and Astronautics, boats and ships weapons, nuclear and electronic apparatus, office machinery, medicine equipment, food, automobile, and occur with material forms such as film, plastics, adhesive, foam, fiber, coatings.As being widely used at present on duplicator, facsimile machine, the scanner.
In recent years, people began to study preparing membrane casing with polyimides.Prior art USP 6,500,375, Dec.31, and 2002, introduced a kind of manufacture method of seamless casing.This method be with biphenyl dianhydride (BPDA) with and the copolymer of p-phenylenediamine (PPD) (PPDA), make polyamic acid resin, make solvent, solutes content 15% with N monomethyl pyrrolidones (NMP) or dimethylacetylamide (DMAC).Improve capacity of heat transmission with boron nitride as filler, the viscosity of polyamic acid resin is between 10000～100000 centipoises.Determine to contain the solution of this weight with the amount of resin of the single sleeve pipe that calculates, with this certain quantity solution by the nozzle ejection or simply be poured on the mandrel of rotation.Use the inclination scraper,, laterally move, solution is blown down on the mandrel uniformly along mandrel by the distance of control scraper and mandrel.The mandrel that will coat resin is removed from lathe then, be transferred to and burn evaporating solvent in the stove, 125 ℃ of constant temperature 1 hour, then mandrel was transferred in 200 ℃ of burning stoves constant temperature 2 hours, afterwards temperature is increased to 250 ℃ of constant temperature 2 hours again, end temperature reaches 380 ℃ of constant temperature 1 hour, is cooled to room temperature, and the Kapton sleeve pipe of formation breaks away from from mandrel.Mandrel is the aluminum cylinder, and external diameter is 25.2 millimeters, and the speed that scraper moves on mandrel meets or exceeds 10 centimeters/minute.This method is compared with the multiple tracks infusion process, and technology is simpler and more direct efficient.But said method, owing to be directly to carry out frictioning on lathe, speed is being generally 10 centimeters/minute, the requirement of incompatibility continuous mass production.And the sample overall dimensions of preparation have certain limitation, to using restriction to some extent.
In addition, the Kapton of method for preparing since be with single biphenyl dianhydride (BPDA) with and the copolymer of making of p-phenylenediamine (PPD) (PPDA), its toughness is relatively poor, tensile strength is bad, lack service life.
Summary of the invention
The object of the present invention is to provide that a kind of good toughness, tensile strength are higher, the heat resisting polyimides amine thin film composite sleeve of long service life.
Another object of the present invention provides a kind ofly can make the method for above-mentioned composite bushing and its production equipment continuously.
The present invention realizes by following measure:
The heat resisting polyimides amine thin film composite sleeve of forming by three-decker of the present invention, its special feature is:
(1) internal layer is the polyimides adhesive film, and thickness is 20～200 microns; Described polyimides adhesive film is made by polyamic acid resin; Described polyamic acid resin is to make with aromatic series dianhydride, aromatic diamine and inorganic filler blending polymerization, and wherein inorganic filler occupies the mass percent of precursor 5～30%;
(2) middle level is that thickness is 5～20 microns a conductive coating;
(3) skin is 10～30 microns fluororesin layer for thickness.
Composite bushing of the present invention, described aromatic series dianhydride are the mixture of pyromellitic acid anhydride (PMDA) and dioxygen ether dianhydride (HQDPA), and its mol ratio is 6～9/4～1; Described aromatic diamine is 4,4 ' one diaminodiphenyl ether (ODA) and benzidine (BZD), and its mol ratio is 1/1; Described inorganic filler be in talcum powder, imvite, silica, molybdenum bisuphide, the boron nitride any or several, its particle diameter is less than 2 microns.
Composite bushing of the present invention, the solvent of described polyamic acid resin are any in dimethyl formamide (DMF), the dimethylacetylamide (DMAC), and the solute percentage by weight in the polyamic acid resin is 16～30%.
Composite bushing of the present invention, described conductive layer are the mixtures of polyamidoimide (pAI) and graphite, conductive carbon black, and wherein the weight ratio of graphite and conductive carbon black is 1/1, accounts for 5～15% of solute percentage by weight.
The preparation method of composite bushing of the present invention may further comprise the steps,
(1) polyamic acid resin being coated in continuously surface brightness is on the minute surface parent tube, its parent tube is that stainless steel tube, aluminum pipe, surface are coated with any in ferrochrome pipe, the polyfluortetraethylene pipe, external diameter is that 5-100 millimeter, length are 200～1000 millimeters column type pipe, and every gluing time is 5-45 second; Automatically defeated then moving carried out slaking in drying tunnel, after the cooling, obtain the Kapton internal layer; Described drying tunnel length is 10-20 rice, and temperature is 60～250 ℃, and temperature increases formula for pursuing;
(2) spray conductive coating on the Kapton internal layer, after the drying, get two layers of multiple tube;
(3) spray fluororesin on the conductive coating; Behind the sintering, obtain described composite bushing.
The equipment that preparation method of the present invention is used, include two positioning modules and a frictioning mouth mould, all has a through hole on same horizontal line on positioning module and the frictioning mouth mould, the aperture of positioning module through hole equals the parent tube external diameter, and the aperture of frictioning mouth mould through hole equals to be coated in the external diameter of the polyamic acid resin film tube on the parent tube.
Heat resisting polyimides amine thin film composite sleeve of the present invention because aromatic series dianhydride, aromatic diamine that the preparation polyimide layer uses are EVA, has good toughness, the advantage of tensile strength height, long service life.
Preparation method of the present invention has gluing speed fast (5～45 seconds/root), and product size scope wide (5～100 millimeters of external diameters, 200～1000 millimeters of length) has realized connection chemical industry production.
It is even that production equipment of the present invention has gluing, one-pass film-forming, the advantage of can serialization producing.
Description of drawings
Accompanying drawing is an automatic double surface gluer schematic diagram of the present invention
Among the figure, 1 one frictioning mouth moulds, 2 one positioning modules, 3 one positioning modules, 4 one parent tubes, 5 one polyimide resins, 6 one direction of propulsion, 7 one glue-lines
The automatic double surface gluer that the present invention adopts is a self design, and as shown in the figure, following mask body is introduced its structure and using method: it is made up of two positioning modules (2,3) and a frictioning mouth mould (1).Polyamic acid resin (5) is joined parent tube (4) position, make the complete submergence of parent tube,, on parent tube, form the uniform ground floor glued membrane of thickness (7), 20～200 microns of thickness through frictioning mouth mould (1) by promoting parent tube along the direction of arrow (6) continuously.Its parent tube is that stainless steel tube, aluminum pipe (or aluminium-alloy pipe) surface are coated with any in ferrochrome pipe, the polyfluortetraethylene pipe, is of a size of external diameter Q5～Q100 millimeter, length and is 200～1000 millimeters column type pipe, and its surface brightness is a minute surface.Every gluing time is 5～45 seconds.Its slaking is to carry out in the drying tunnel that rotation is carried forward, and whole drying tunnel length is 10～20 meters, and temperature is 60～250 ℃.
On the ground floor basement membrane, carry out the conductive layer spraying, thickness is 5～20 microns, forms two layers of composite bushing.Conductive layer is that wherein the weight ratio of graphite and conductive carbon black is 1/1, accounts for 5～15% of solute percentage by weight by the mixture of polyamidoimide (PAI) and graphite, conductive carbon black.
Carry out the spraying of fluororesin or its water paint on two layers of composite bushing that form, behind sintering, make the laminated film sleeve pipe that contains trilaminate material, wherein trilamellar membrane is thick 10～30 microns.
According to the Kapton composite bushing of the present invention's preparation, its second layer sheet resistance is 10
6～10
10Ω cm.
The specific embodiment
For better implement the present invention,, but not limitation of the present invention especially exemplified by the example explanation.
Embodiment 1
1308 gram (6 moles) pyromellitic acid anhydrides (PMDA) and 1608 gram (4 moles) dioxygen ether dianhydrides (HQDPA), 1000 gram (5 moles) 4,4 '-diaminodiphenyl ether (ODA) and 920 gram (5 moles) benzidines (BZD), 25389 gram dimethyl acetic acid glue (DMAc) (solid content 16%), 4836 gram talcum powder add reactor together, stir after 2 hours under the room temperature, be heated to 60 ℃ and continue reaction 6 hours, make polyamic acid resin.Carry out continuous gluing with stainless steel tube (8 millimeters of external diameter ￠, 220 millimeters of length) on glue spreading apparatus, gluing speed is 5 seconds/root, obtains uniform glue-line.Carry out slaking in 10 meters long rotations conveying drying tunnel, initial temperature is 60 ℃, and progressively heating up is heated to 250 ℃, after the cooling, obtains the ground floor basement membrane, and thickness is 20 microns.Polyamidoimide with 30% (PAI) 700 gram wherein adds 7.5 gram graphite, 7.5 gram conductive carbon blacks (accounting for solute weight 5%) spray, and obtain two layers of composite bushing after the drying.Wherein second layer thickness is 6 microns, sheet resistance 4.5 * 10
9Ω cm.Spray with the polytetrafluoroethylene (PTFE) emulsion at last, behind sintering, obtain containing the thin film composite sleeve of trilaminate material.Outermost layer thickness is 10 microns.
Embodiment 2
1635 gram (7.5 moles) pyromellitic acid anhydrides and 1005 gram (2.5 moles) dioxygen ether dianhydrides, 4, the addition of 4 ' one diaminodiphenyl ether and benzidine and embodiment are 1 identical, 23940 gram dimethylacetylamides (solid content 16%), 2280 gram imvites, aluminum pipe (15 millimeters of external diameter ￠, 300 millimeters of length) gluing speed are 8 seconds/root, adopt the manufacturing technique method identical to make polyamic acid resin and gluing with embodiment 1, obtain the ground floor basement membrane, thickness is 40 microns.Polyamidoimide with 30% (PAI) 700 gram wherein adds 12 gram graphite, 12 gram conductive carbon blacks spray, and obtain two layers of composite bushing after the drying.Wherein second layer thickness is 10 microns, sheet resistance 3.1 * 10
8Ω cm.Use Meltability polytetrafluorethyletubular (PFA) emulsion to spray at last, behind the sintering, obtain containing the thin film composite sleeve of trilaminate material.15 microns of outermost layer thickness.
Embodiment 3
1962 gram (9 moles) pyromellitic acid anhydrides and 402 gram (1 mole) dioxygen ether dianhydrides, 4, the addition of 4 '-diaminodiphenyl ether and benzidine and embodiment are 1 identical, 22491 gram dimethylacetylamides (solid content 16%), 1535 gram boron nitride, polyfluortetraethylene pipe (40 millimeters of external diameter ￠, 400 millimeters of length), gluing speed are 15 seconds/root, adopt the manufacturing technique method identical to make polyamic acid resin and gluing with embodiment 1, obtain the ground floor basement membrane, thickness is 60 microns.Polyamidoimide with 30% (PA1) 700 gram wherein adds 15 gram graphite, 15 gram conductive carbon blacks spray, and obtain two layers of composite bushing after the drying.Wherein second layer thickness is 15 microns, sheet resistance 6.3 * 10
7Ω cm.Use Meltability polytetrafluorethyletubular (PFA) emulsion to spray at last, behind the sintering, obtain containing the thin film composite sleeve of trilaminate material.20 microns of outermost layer thickness.
Embodiment 4
1962 gram (9 moles) pyromellitic acid anhydrides and 402 gram (1 mole) dioxygen ether dianhydrides, 4, the addition of 4 ' one diaminodiphenyl ether and benzidine with implement ice-cold 1 identical, 13566 gram dimethylacetylamides (solid content 24%), 950 gram silica, surface and be coated with ferrochrome pipe (35 millimeters of external diameter ￠, 350 millimeters of length), 21 seconds/root of gluing speed, 15 meters drying tunnels, adopt the manufacturing technique method identical to make polyamic acid resin and gluing with embodiment 1, obtain the ground floor basement membrane, thickness is 85 microns.Polyamidoimide with 30% (PA1) 700 gram wherein adds 15 gram graphite, 15 gram conductive carbon blacks spray, and obtain two layers of composite bushing after the drying.Wherein second layer thickness is 20 microns, sheet resistance 5.0 * 10
7Ω cm.Use Meltability polytetrafluorethyletubular (PFA) emulsion to spray at last, behind the sintering, obtain containing the thin film composite sleeve of trilaminate material.25 microns of outermost layer thickness.
Embodiment 5
1635 gram (7.5 moles) pyromellitic acid anhydrides and 1005 gram (2.5 moles) dioxygen ether dianhydrides 4, the addition of 4 ' one diaminodiphenyl ether and benzidine is identical with embodiment 1.14440 gram dimethylacetylamides (solid content 24%), 1900 gram molybdenum bisuphide, stainless steel tube (60 millimeters of external diameter ￠, 500 millimeters of length), gluing speed are 25 seconds/root, 15 meters drying tunnels, adopt the manufacturing technique method identical to make polyamic acid resin and gluing with embodiment 1, obtain the ground floor basement membrane, thickness is 100 microns.With 30% poly-swash amino acid imines (PAI) 700 grams, wherein add 18 gram graphite, 18 gram conductive carbon blacks spray, and obtain two layers of composite bushing after the drying.Wherein second layer thickness is 25 microns, sheet resistance 8.5 * 10
6Ω cm.Use Meltability polytetrafluorethyletubular (PFA) emulsion to spray at last, behind the sintering, obtain containing the thin film composite sleeve of trilaminate material.25 microns of outermost layer thickness.
Embodiment 6
1308 gram (6 moles) pyromellitic acid anhydrides and 1608 gram (4 moles) dioxygen ether dianhydrides 4, the addition of 4 ' one diaminodiphenyl ether and benzidine and embodiment are 1 identical, 15314 gram dimethylacetylamides (solid content 24%), 1100 gram imvites, aluminum pipe (55 millimeters of external diameter ￠, 450 millimeters of length) gluing speed are 24 seconds/root, 15 meters drying tunnels, adopt the manufacturing technique method identical to make polyamic acid resin and gluing with example I, obtain the ground floor basement membrane, thickness is 90 microns.Polyamidoimide with 30% (PAI) 700 gram wherein adds 10 gram graphite, 10 gram conductive carbon blacks spray, and obtain two layers of composite bushing after the drying.Wherein second layer thickness is 20 microns, sheet resistance 2.3 * 10
8Ω cm.Spray with the polytetrafluoroethylene (PTFE) emulsion at last, behind the sintering, obtain containing the thin film composite sleeve of trilaminate material.20 microns of outermost layer thickness.
Embodiment 7
1308 gram (6 moles) pyromellitic acid anhydrides and 1608 gram (4 moles) dioxygen ether dianhydrides, 4, the addition of two ethers of 4 '-diaminourea and benzidine and embodiment are 1 identical, to be coated with ferrochrome pipe (100 millimeters of external diameter ￠, 1000 millimeters of length) gluing speed be 45 seconds/root, 20 meters drying tunnels for 11284 gram dimethyl formamides (DMF) (solid content 30%), 6900 gram talcum powder, surface, adopt the manufacturing technique method identical to make polyamic acid resin and gluing with embodiment 1, obtain the ground floor basement membrane, thickness is 200 microns.Polyamidoimide with 30% (PAI) 700 gram wherein adds 10 gram graphite, 10 gram conductive carbon blacks spray, and obtain two layers of composite bushing after the drying.Wherein second layer thickness is 5 microns, sheet resistance 2.3 * 10 ' Ω cm.Spray with the polytetrafluoroethylene (PTFE) emulsion at last, behind the sintering, obtain containing the thin film composite sleeve of trilaminate material.5 microns of outermost layer thickness.
Embodiment 8
1635 gram (6 moles) pyromellitic acid anhydrides and 1005 gram (4 moles) dioxygen ether dianhydrides, 4, the addition of 4 ' diaminodiphenyl ether and benzidine and embodiment are 1 identical, 10640 gram dimethyl formamides (DMF) (solid content 30%), 1370 gram silica, polyfluortetraethylene pipe (60 millimeters of external diameter ￠, 600 millimeters of length) gluing speed are 35 seconds/root, 20 meters drying tunnels, adopt the manufacturing technique method identical to make polyamic acid resin and gluing with embodiment 1, obtain the ground floor basement membrane, thickness is 100 microns.Polyamidoimide with 30% (PAI) 700 gram wherein adds 12 gram graphite, 12 gram conductive carbon blacks spray, and obtain two layers of composite bushing after the drying.Wherein second layer thickness is 15 microns, vindication resistance 7.9 * 10
8Ω cm.Use fusible polytetrafluoroethylene (PTFE) (PFA) emulsion to spray at last, behind the sintering, obtain containing the thin film composite sleeve of trilaminate material.15 microns of outermost layer thickness.
Embodiment 9
1962 gram (6 moles) pyromellitic acid anhydrides and 402 gram (4 moles) dioxygen ether dianhydrides, 4, the addition of 4 ' diaminodiphenyl ether and benzidine and embodiment are 1 identical, 9996 gram dimethyl formamides (DMF) (solid content 30%), 1720 gram boron nitride, aluminum pipe (40 millimeters of external diameter Ф, 400 millimeters of length), gluing speed are 23 seconds/root, 20 meters drying tunnels, adopt the manufacturing technique method identical to make polyamic acid resin and gluing with embodiment 1, obtain the ground floor basement membrane, thickness is 60 microns.Polyamidoimide with 30% (PAI) 700 gram wherein adds 10 gram graphite, 10 gram conductive carbon blacks spray, and obtain two layers of composite bushing after the drying.Wherein second layer thickness is 12 microns, sheet resistance 1.6 * 10
8After Ω cm. uses Meltability polytetrafluorethyletubular (PFA) emulsion to carry out spray sintering at last, obtain containing the thin film composite sleeve of trilaminate material.12 microns of outermost layer thickness.
Claims (6)
1, a kind of heat resisting polyimides amine thin film composite sleeve of being made up of three-decker is characterized in that:
(1) internal layer is the polyimides adhesive film, and thickness is 20～200 microns; Described polyimides adhesive film is made by polyamic acid resin; Described polyamic acid resin is to make with aromatic series dianhydride, aromatic diamine and inorganic filler blending polymerization, and wherein inorganic filler occupies the mass percent of precursor 5～30%;
(2) middle level is that thickness is 5～20 microns a conductive coating;
(3) skin is 10～30 microns fluororesin layer for thickness.
2, heat resisting polyimides amine thin film composite sleeve according to claim 1 is characterized in that: described aromatic series dianhydride is the mixture of pyromellitic acid anhydride (PMDA) and dioxygen ether dianhydride (HQDPA), and its mol ratio is 6～9/4～1; Described aromatic diamine is 4,4 ' one diaminodiphenyl ether (ODA) and benzidine (BZD), and its mol ratio is 1/1; Described inorganic filler be in talcum powder, imvite, silica, molybdenum bisuphide, the boron nitride any or several, its particle diameter is less than 2 microns.
3, heat resisting polyimides amine thin film composite sleeve according to claim 1 and 2, it is characterized in that: the solvent of described polyamic acid resin is any in dimethyl formamide (DMF), the dimethylacetylamide (DMAC), and the solute percentage by weight in the polyamic acid resin is 16～30%.
4, heat resisting polyimides amine thin film composite sleeve according to claim 1 and 2, it is characterized in that: described conductive layer is the mixture of polyamidoimide (pAI) and graphite, conductive carbon black, wherein the weight ratio of graphite and conductive carbon black is 1/1, accounts for 5～15% of solute percentage by weight.
5, the preparation method of the described heat resisting polyimides amine of a kind of claim 1 thin film composite sleeve is characterized in that: may further comprise the steps,
(1) polyamic acid resin is coated in continuously on the parent tube that surface brightness is a minute surface, its parent tube is that stainless steel tube, aluminum pipe, surface are coated with any in ferrochrome pipe, the polyfluortetraethylene pipe, external diameter is that 5-100 millimeter, length are 200～1000 millimeters column type pipe, and every gluing time is 5-45 second; Automatically defeated then moving carried out slaking in drying tunnel, after the cooling, obtain the Kapton internal layer; Described drying tunnel length is 10-20 rice, and temperature is 60～250 ℃, and temperature increases formula for pursuing;
(2) spray conductive coating on the Kapton internal layer, after the drying, get two layers of multiple tube;
(3) spray fluororesin on the conductive coating; Behind the sintering, obtain described composite bushing.
6, a kind of used equipment of 1 described preparation method that requires of planting of weighing, it is characterized in that: include two positioning modules and a frictioning mouth mould, all has a through hole on same horizontal line on positioning module and the frictioning mouth mould, the aperture of positioning module through hole equals the parent tube external diameter, and the aperture of frictioning mouth mould through hole equals to be coated in the external diameter of the polyamic acid resin film tube on the parent tube.
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| CN 200410024495 CN1226137C (en) | 2004-07-13 | 2004-07-13 | Heat resistant polyimide film composite casing pipe, preparation method and equipment thereof |
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| CN 200410024495 CN1226137C (en) | 2004-07-13 | 2004-07-13 | Heat resistant polyimide film composite casing pipe, preparation method and equipment thereof |
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| CN1593908A true CN1593908A (en) | 2005-03-16 |
| CN1226137C CN1226137C (en) | 2005-11-09 |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102522167A (en) * | 2011-12-30 | 2012-06-27 | 天津市华之阳特种线缆有限公司 | Polyimide coiled sleeve and processing method thereof |
| CN102522165A (en) * | 2011-12-30 | 2012-06-27 | 天津市华之阳特种线缆有限公司 | H-class composite protection sleeve for winding of motor of refrigeration compressor |
| CN102950868A (en) * | 2011-08-16 | 2013-03-06 | 富士施乐株式会社 | Method for manufacturing endless belt |
| CN103738023A (en) * | 2014-01-20 | 2014-04-23 | 苏州新区特氟龙塑料制品厂 | Teflon film |
| CN104530703A (en) * | 2015-01-20 | 2015-04-22 | 无锡顺铉新材料有限公司 | Low-dielectric constant polyimide and preparation method thereof |
| CN112316736A (en) * | 2020-10-26 | 2021-02-05 | 武汉工程大学 | Method for preparing tubular composite membrane by limited space phase inversion, external coating device, internal coating device and composite membrane |
-
2004
- 2004-07-13 CN CN 200410024495 patent/CN1226137C/en not_active Expired - Fee Related
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102950868A (en) * | 2011-08-16 | 2013-03-06 | 富士施乐株式会社 | Method for manufacturing endless belt |
| CN102522167A (en) * | 2011-12-30 | 2012-06-27 | 天津市华之阳特种线缆有限公司 | Polyimide coiled sleeve and processing method thereof |
| CN102522165A (en) * | 2011-12-30 | 2012-06-27 | 天津市华之阳特种线缆有限公司 | H-class composite protection sleeve for winding of motor of refrigeration compressor |
| CN102522165B (en) * | 2011-12-30 | 2014-12-17 | 天津市华之阳特种线缆有限公司 | H-class composite protection sleeve for winding of motor of refrigeration compressor |
| CN102522167B (en) * | 2011-12-30 | 2015-08-26 | 天津市华之阳特种线缆有限公司 | Polyimide coiled sleeve and processing method thereof |
| CN103738023A (en) * | 2014-01-20 | 2014-04-23 | 苏州新区特氟龙塑料制品厂 | Teflon film |
| CN104530703A (en) * | 2015-01-20 | 2015-04-22 | 无锡顺铉新材料有限公司 | Low-dielectric constant polyimide and preparation method thereof |
| CN112316736A (en) * | 2020-10-26 | 2021-02-05 | 武汉工程大学 | Method for preparing tubular composite membrane by limited space phase inversion, external coating device, internal coating device and composite membrane |
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|---|---|
| CN1226137C (en) | 2005-11-09 |
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