CN105936693A - Waterproof, impervious, and heatproof optical fiber material and preparation method thereof - Google Patents
Waterproof, impervious, and heatproof optical fiber material and preparation method thereof Download PDFInfo
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- CN105936693A CN105936693A CN201610457151.9A CN201610457151A CN105936693A CN 105936693 A CN105936693 A CN 105936693A CN 201610457151 A CN201610457151 A CN 201610457151A CN 105936693 A CN105936693 A CN 105936693A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L23/00—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers
- C08L23/02—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers not modified by chemical after-treatment
- C08L23/04—Homopolymers or copolymers of ethene
- C08L23/06—Polyethene
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G73/00—Macromolecular compounds obtained by reactions forming a linkage containing nitrogen with or without oxygen or carbon in the main chain of the macromolecule, not provided for in groups C08G12/00 - C08G71/00
- C08G73/06—Polycondensates having nitrogen-containing heterocyclic rings in the main chain of the macromolecule
- C08G73/10—Polyimides; Polyester-imides; Polyamide-imides; Polyamide acids or similar polyimide precursors
- C08G73/1067—Wholly aromatic polyimides, i.e. having both tetracarboxylic and diamino moieties aromatically bound
- C08G73/1071—Wholly aromatic polyimides containing oxygen in the form of ether bonds in the main chain
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/08—Stabilised against heat, light or radiation or oxydation
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2203/00—Applications
- C08L2203/20—Applications use in electrical or conductive gadgets
- C08L2203/202—Applications use in electrical or conductive gadgets use in electrical wires or wirecoating
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2207/00—Properties characterising the ingredient of the composition
- C08L2207/06—Properties of polyethylene
- C08L2207/062—HDPE
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Abstract
The invention discloses a waterproof, impervious, and heatproof optical fiber material, which is composed of the following components in parts by weight: 0.6 to 1 part of dibenzothiazyl disulfide, 5 to 7 parts of octamethyl cyclotetrasiloxane, 2 to 3 parts of octaphenyl-POSS, 0.01 to 0.02 part of tetramethyl ammonium hydroxide, 300 to 400 parts of dimethyl acetamide, 1 to 3 parts of octyl phenyl cyclotetrasiloxane, 37 to 40 parts of 4,4'-diaminodiphenyl ether, 2 to 4 parts of ammonia liquor (20-25%), 46 to 50 parts of pyromellitic dianhydride, 70 to 80 parts of N-methyl pyrrolidone, 3 to 4 parts of aluminum nitride, 100 to 110 parts of high density polyethylene, 1 to 1.6 parts of fatty acid diethanol amide, 2.5 to 4 parts of allyl alcohol, 1 to 3 parts of manganese oxide, 3 to 5 parts of epoxy triglyceride, 1 to 2 parts of molybdenum disulfide, 0.3 to 1 part of alkenyl succinic anhydride, and 4 to 5 parts of dimethyl formamide. The provided optical cable material has a good waterproof and impervious performance and is resistant to dampness and heat.
Description
Technical field
The present invention relates to mass technical field, particularly relate to a kind of water proof anti-seepage heat-resistant cable material and preparation method thereof.
Background technology
nullComposite polyimide material is generally composited with polyimides for matrix and other material " wherein with poly-phthalimide for matrix with high performance reinforcing fiber (such as glass fibre，Carbon fiber，Aramid fiber etc.) advanced composite material that is composited，Specific strength is high，High temperature resistant，Part weight is light，It is largely used to make the structural member of aerospace vehicle，It is " current with polyimides as matrix that huge contribution has been made in development to aerospace industry，The research compound with inorganic particles is more and more noticeable，As functional composite material，Having broad prospect of application " mainly has pottery for the inorganic matter of polyimide/inorganic thing (nanometer) composite and the material of precursor thereof、Polysiloxanes、Clay and molecular sieve，Generally inorganic matter is scattered in polyimide matrix with the form of dispersion phase，" inorganic matter can be with in the form introducing polyimides of superfine powder to form the inorganic phase of certain size that is separated，More generally it is then converted to corresponding inorganic phase so that certain precursor form (such as alkoxide etc.) and the precursor solution of polyimides are blended；
Owing to general polyimides does not melts, processing and forming temperature is high, therefore exploitation is prone to the focus that the polyimides of processing and forming is its research and development, and " polyimides that in addition; owing to it is relatively costly; be greatly limited in terms of general civilian and commercial Application; therefore synthesize low cost, property retention is good is also one of emphasis of studying；
Polyimides has the most excellent thermostability, wearability, radiation resistance, chemical resistance, good electrical insulating property, toughness, the most also there is the highest gas permeability, owing to having superior combination property, it is widely used in Aero-Space, electric, locomotive automobile, the field such as precision optical machinery and automatic office machinery, polyimide curing temperature is the highest, and is difficult to processing and forming, and polyimides is prepared as powder, then can have the most wide application prospect as material modification additive；.
Summary of the invention
The object of the invention is contemplated to make up the defect of prior art, it is provided that a kind of water proof anti-seepage heat-resistant cable material and preparation method thereof.
The present invention is achieved by the following technical solutions:
A kind of water proof anti-seepage heat-resistant cable material, it is made up of the raw material of following weight parts:
Dibenzothiazyl disulfide 0.6-1, octamethylcy-clotetrasiloxane 5-7, octaphenyl-POSS2-3, Tetramethylammonium hydroxide 0.01-0.02, dimethyl acetylamide 300-400, octyl phenyl cyclotetrasiloxane 1-3, 4, 4'-diaminodiphenyl ether 37-40, the ammonia 2-4 of 20-25%, pyromellitic acid anhydride 46-50, N-Methyl pyrrolidone 70-80, aluminium nitride 3-4, high density polyethylene (HDPE) 100-110, fatty diglycollic amide 1-1.6, propenyl 2.5-4, manganese oxide 1-3, epoxidation triglyceride 3-5, molybdenum bisuphide 1-2, alkenyl succinic anhydride 0.3-1, dimethylformamide 4-5.
The preparation method of a kind of described water proof anti-seepage heat-resistant cable material, comprises the following steps:
(1) taking the 10-15% of above-mentioned octamethylcy-clotetrasiloxane weight, mix with Tetramethylammonium hydroxide, be passed through nitrogen, insulation reaction 2-3 hour at 90-95 DEG C, slowly reducing temperature is room temperature, obtains alkaline-sol；
(2) above-mentioned dibenzothiazyl disulfide is joined in dimethylformamide, insulated and stirred 3-7 minute at 50-60 DEG C, add the 10-15% of above-mentioned dimethyl acetylamide weight, stirring, to room temperature, obtains compound amide solution；
(3) take above-mentioned compound amide solution, add remaining octamethylcy-clotetrasiloxane, octyl phenyl cyclotetrasiloxane, octaphenyl-POSS, stir, it is passed through nitrogen, add above-mentioned alkaline-sol, 90-95 DEG C of insulated and stirred 30-40 minute, stop being passed through nitrogen, it is incubated 2-3 hour, rise high-temperature and be 150-160 DEG C, be incubated 27-30 minute, cooling, it is vacuum dried 1-2 hour at 60-65 DEG C, obtains cross linking polysiloxane；
(4) by above-mentioned 4,4'-diaminodiphenyl ether joins in its weight 36-40 times, 15-17% sulfuric acid solution, adds the ammonia of above-mentioned 20-25%, stand 1-2 hour, filter, precipitate with deionized water is washed 3-4 time, it is vacuum dried 4-5 hour at 60-70 DEG C, obtains refined phenylate；
(5) above-mentioned fatty diglycollic amide is joined in the deionized water of its weight 27-30 times, stir, add manganese oxide, molybdenum bisuphide, ultrasonic 3-5 minute, obtain aqueous dispersions；
(6) by above-mentioned refined phenylate, pyromellitic acid anhydride, cross linking polysiloxane mixing, add remaining dimethyl acetylamide, stir, send in ice-water bath, it is passed through nitrogen, stirring reaction 2-3 hour, adds above-mentioned alkenyl succinic anhydride, stir, discharging, joins product in aqueous dispersions, and room temperature stands 4-5 days, filter, obtain precrosslink polyimides；
(7) above-mentioned aluminium nitride is joined in N-Methyl pyrrolidone, ultrasonic 2-3 minute, obtain aluminium nitride dispersion liquid；
(8) above-mentioned precrosslink polyimides is joined in aluminium nitride dispersion liquid, ultrasonic 20-30 minute, filter, it will be vacuum dried 3-5 hour at being deposited in 76-80 DEG C, wears into fine powder, send in the vacuum drying oven of 250-260 DEG C, heating 6-7 hour, discharging cools down, and obtains cross-linking modified polyimides；
(9) by above-mentioned cross-linking modified polyimides, propenyl, the mixing of epoxidation triglyceride, rise high-temperature and be 70-80 DEG C, insulated and stirred 3-5 minute, mix with remaining each raw material, stir, be sent in screw extruder, melt extrude, cooling, pulverizing, obtain described mass.
The invention have the advantage that the present invention is with 4,4. a diaminodiphenyl ether and pyromellitic acid anhydride are monomer, with N-Methyl pyrrolidone as reaction dissolvent, with cross linking polysiloxane as hydrophobic components, remove solvent through distilled water immersion after having reacted, then high temperature cyclization obtains cross-linking modified polyimides；
The present invention introduces in the strand of polyimides has hydrophobic Si-O-Si structure, by the polyimides shearing force to cross linking polysiloxane, polysiloxanes can be dispersed into less granule, it can be uniformly coated on the surface of polyimide particle, thus form hydrophobic layer, thus improve its dispersing uniformity in the composite；The cross linking polysiloxane of the present invention also has good heat stability and irradiation stability, improves its damping capacity and the compatibility with polyimides；Precrosslink polyimides is mixed by the present invention with aluminium nitride suspension, and the composite of formation combines the respective advantage of polyimides and aluminium nitride, has high heat conduction, low bulk, low dielectric, electric insulation, the high temperature resistant performance waiting excellence；The mass of the present invention has good water impermeability, and humidity resistance is good.
Detailed description of the invention
A kind of water proof anti-seepage heat-resistant cable material, it is made up of the raw material of following weight parts:
Dibenzothiazyl disulfide 0.6, octamethylcy-clotetrasiloxane 5, octaphenyl POSS2, Tetramethylammonium hydroxide 0.01, dimethyl acetylamide 300, octyl phenyl cyclotetrasiloxane 1,4, the ammonia 2 of 4' diaminodiphenyl ether 37,20%, pyromellitic acid anhydride 46, N methyl pyrrolidone 70, aluminium nitride 3, high density polyethylene (HDPE) 100, fatty diglycollic amide 1, propenyl 2.5, manganese oxide 1, epoxidation triglyceride 3, molybdenum bisuphide 1, alkenyl succinic anhydride 0.3, dimethylformamide 4.
The preparation method of a kind of described water proof anti-seepage heat-resistant cable material, comprises the following steps:
(1) taking the 10% of above-mentioned octamethylcy-clotetrasiloxane weight, mix with Tetramethylammonium hydroxide, be passed through nitrogen, insulation reaction 2 hours at 90 DEG C, slowly reducing temperature is room temperature, obtains alkaline-sol；
(2) above-mentioned dibenzothiazyl disulfide is joined in dimethylformamide, insulated and stirred 3 minutes at 50 DEG C, add the 10% of above-mentioned dimethyl acetylamide weight, stirring, to room temperature, obtains compound amide solution；
(3) take above-mentioned compound amide solution, add remaining octamethylcy-clotetrasiloxane, octyl phenyl cyclotetrasiloxane, octaphenyl POSS, stir, it is passed through nitrogen, add above-mentioned alkaline-sol, 90 DEG C of insulated and stirred 30 minutes, stop being passed through nitrogen, it is incubated 2 hours, rising high-temperature is 150 DEG C, is incubated 27 minutes, cooling, it is vacuum dried 1 hour at 60 DEG C, obtains cross linking polysiloxane；
(4) by above-mentioned 4,4' diaminodiphenyl ether joins in its weight 36 times, the sulfuric acid solution of 15%, adds the ammonia of above-mentioned 20%, stands 1 hour, filters, precipitate with deionized water is washed 3 times, is vacuum dried 4 hours, obtains refined phenylate at 60 DEG C；
(5) above-mentioned fatty diglycollic amide is joined in the deionized water of its weight 27 times, stir, add manganese oxide, molybdenum bisuphide, ultrasonic 3 minutes, obtain aqueous dispersions；
(6) by above-mentioned refined phenylate, pyromellitic acid anhydride, cross linking polysiloxane mixing, add remaining dimethyl acetylamide, stir, send in ice-water bath, it is passed through nitrogen, stirring reaction 2 hours, adds above-mentioned alkenyl succinic anhydride, stir, discharging, joins product in aqueous dispersions, and room temperature stands 4 days, filter, obtain precrosslink polyimides；
(7) above-mentioned aluminium nitride is joined in N methyl pyrrolidone, ultrasonic 2 minutes, obtain aluminium nitride dispersion liquid；
(8) above-mentioned precrosslink polyimides is joined in aluminium nitride dispersion liquid, ultrasonic 20 minutes, filter, vacuum drying 3 hours will be deposited at 76 DEG C, wear into fine powder, send in the vacuum drying oven of 250 DEG C, heating 6 hours, discharging cools down, and obtains cross-linking modified polyimides；
(9) by above-mentioned cross-linking modified polyimides, propenyl, the mixing of epoxidation triglyceride, rising high-temperature is 70 DEG C, insulated and stirred 3 minutes, mixes with remaining each raw material, stir, be sent in screw extruder, melt extrude, cooling, pulverizing, obtain described mass.
Performance test:
Hot strength: 19.6 MPa；
Elongation at break: 350%.
Claims (2)
1. a water proof anti-seepage heat-resistant cable material, it is characterised in that it is made up of the raw material of following weight parts:
Dibenzothiazyl disulfide 0.6-1, octamethylcy-clotetrasiloxane 5-7, octaphenyl-POSS2-3, Tetramethylammonium hydroxide 0.01-0.02, dimethyl acetylamide 300-400, octyl phenyl cyclotetrasiloxane 1-3, 4, 4'-diaminodiphenyl ether 37-40, the ammonia 2-4 of 20-25%, pyromellitic acid anhydride 46-50, N-Methyl pyrrolidone 70-80, aluminium nitride 3-4, high density polyethylene (HDPE) 100-110, fatty diglycollic amide 1-1.6, propenyl 2.5-4, manganese oxide 1-3, epoxidation triglyceride 3-5, molybdenum bisuphide 1-2, alkenyl succinic anhydride 0.3-1, dimethylformamide 4-5.
2. the preparation method of a water proof anti-seepage heat-resistant cable material as claimed in claim 1, it is characterised in that comprise the following steps:
(1) taking the 10-15% of above-mentioned octamethylcy-clotetrasiloxane weight, mix with Tetramethylammonium hydroxide, be passed through nitrogen, insulation reaction 2-3 hour at 90-95 DEG C, slowly reducing temperature is room temperature, obtains alkaline-sol；
(2) above-mentioned dibenzothiazyl disulfide is joined in dimethylformamide, insulated and stirred 3-7 minute at 50-60 DEG C, add the 10-15% of above-mentioned dimethyl acetylamide weight, stirring, to room temperature, obtains compound amide solution；
(3) take above-mentioned compound amide solution, add remaining octamethylcy-clotetrasiloxane, octyl phenyl cyclotetrasiloxane, octaphenyl-POSS, stir, it is passed through nitrogen, add above-mentioned alkaline-sol, 90-95 DEG C of insulated and stirred 30-40 minute, stop being passed through nitrogen, it is incubated 2-3 hour, rise high-temperature and be 150-160 DEG C, be incubated 27-30 minute, cooling, it is vacuum dried 1-2 hour at 60-65 DEG C, obtains cross linking polysiloxane；
(4) by above-mentioned 4,4'-diaminodiphenyl ether joins in its weight 36-40 times, 15-17% sulfuric acid solution, adds the ammonia of above-mentioned 20-25%, stand 1-2 hour, filter, precipitate with deionized water is washed 3-4 time, it is vacuum dried 4-5 hour at 60-70 DEG C, obtains refined phenylate；
(5) above-mentioned fatty diglycollic amide is joined in the deionized water of its weight 27-30 times, stir, add manganese oxide, molybdenum bisuphide, ultrasonic 3-5 minute, obtain aqueous dispersions；
(6) by above-mentioned refined phenylate, pyromellitic acid anhydride, cross linking polysiloxane mixing, add remaining dimethyl acetylamide, stir, send in ice-water bath, it is passed through nitrogen, stirring reaction 2-3 hour, adds above-mentioned alkenyl succinic anhydride, stir, discharging, joins product in aqueous dispersions, and room temperature stands 4-5 days, filter, obtain precrosslink polyimides；
(7) above-mentioned aluminium nitride is joined in N-Methyl pyrrolidone, ultrasonic 2-3 minute, obtain aluminium nitride dispersion liquid；
(8) above-mentioned precrosslink polyimides is joined in aluminium nitride dispersion liquid, ultrasonic 20-30 minute, filter, it will be vacuum dried 3-5 hour at being deposited in 76-80 DEG C, wears into fine powder, send in the vacuum drying oven of 250-260 DEG C, heating 6-7 hour, discharging cools down, and obtains cross-linking modified polyimides；
(9) by above-mentioned cross-linking modified polyimides, propenyl, the mixing of epoxidation triglyceride, rise high-temperature and be 70-80 DEG C, insulated and stirred 3-5 minute, mix with remaining each raw material, stir, be sent in screw extruder, melt extrude, cooling, pulverizing, obtain described mass.
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| CN201610457151.9A CN105936693A (en) | 2016-06-22 | 2016-06-22 | Waterproof, impervious, and heatproof optical fiber material and preparation method thereof |
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| CN201610457151.9A CN105936693A (en) | 2016-06-22 | 2016-06-22 | Waterproof, impervious, and heatproof optical fiber material and preparation method thereof |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106566144A (en) * | 2016-10-19 | 2017-04-19 | 安徽吉思特智能装备有限公司 | Aluminium sol high-dielectric material and preparation method thereof |
| CN115044274A (en) * | 2022-07-19 | 2022-09-13 | 宁波科鑫腐蚀控制工程有限公司 | Ceramic particle modified fiber epoxy composite coating and preparation method and application thereof |
Citations (1)
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| CN1837262A (en) * | 2006-04-24 | 2006-09-27 | 广州吉必时科技实业有限公司 | Process for synthesis of polysiloxane |
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2016
- 2016-06-22 CN CN201610457151.9A patent/CN105936693A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1837262A (en) * | 2006-04-24 | 2006-09-27 | 广州吉必时科技实业有限公司 | Process for synthesis of polysiloxane |
Non-Patent Citations (2)
| Title |
|---|
| 张飞: "聚酰亚胺/聚硅氧烷复合微粒子的制备与性质研究", 《中国优秀硕士学位论文全文数据库工程科技Ⅰ辑》 * |
| 谢元等: "高密度聚乙烯电缆护套料的研制", 《化工新型材料》 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106566144A (en) * | 2016-10-19 | 2017-04-19 | 安徽吉思特智能装备有限公司 | Aluminium sol high-dielectric material and preparation method thereof |
| CN115044274A (en) * | 2022-07-19 | 2022-09-13 | 宁波科鑫腐蚀控制工程有限公司 | Ceramic particle modified fiber epoxy composite coating and preparation method and application thereof |
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Application publication date: 20160914 |