CN105936695A - Aluminum nitride enhanced heatproof optical cable material and preparation method thereof - Google Patents
Aluminum nitride enhanced heatproof optical cable material and preparation method thereof Download PDFInfo
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- CN105936695A CN105936695A CN201610457181.XA CN201610457181A CN105936695A CN 105936695 A CN105936695 A CN 105936695A CN 201610457181 A CN201610457181 A CN 201610457181A CN 105936695 A CN105936695 A CN 105936695A
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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
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- 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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- C08G77/00—Macromolecular compounds obtained by reactions forming a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon in the main chain of the macromolecule
- C08G77/04—Polysiloxanes
- C08G77/06—Preparatory processes
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- C08L2201/08—Stabilised against heat, light or radiation or oxydation
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- C08L2207/00—Properties characterising the ingredient of the composition
- C08L2207/06—Properties of polyethylene
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Abstract
The invention discloses an aluminum nitride enhanced heatproof optical cable material, which is composed of the following raw materials in parts by weight: 0.1 to 0.2 part of 2,4-imidazolinedione, 0.1 to 0.3 part of tripropylene glycol methyl ether, 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, 3 to 4 parts of dibutyl phthalate, 1 to 2 parts of polyisobutylene, 0.8 to 1 part of zinc pyrithione, 3 to 4 parts of silicon carbide, and 0.1 to 0.2 part of trimethyl hydroxyethyl ethylene diamine. The provided optical cable material has the advantages of excellent performance on resisting acid, alkali, wet, and heat, high surface strength, and good toughness.
Description
Technical field
The present invention relates to mass technical field, particularly relate to a kind of aluminium nitride and strengthen 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 aluminium nitride strengthens heat-resistant cable material and preparation method thereof.
The present invention is achieved by the following technical solutions:
A kind of aluminium nitride strengthens heat-resistant cable material, and it is made up of the raw material of following weight parts:
2, 4-imidazolinedione 0.1-0.2, tripropylene glycol methyl ether 0.1-0.3, 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, phthalic acid dibutyl ester 3-4, polyisobutylene 1-2, Zinc Pyrithione 0.8-1, carborundum 3-4, trimethyl hydroxyethylammonium ethylenediamine 0.1-0.2.
A kind of described aluminium nitride strengthens the preparation method of 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) take the 10-15% of above-mentioned dimethyl acetylamide weight, add above-mentioned Zinc Pyrithione, ultrasonic 2-3 minute, add remaining octamethylcy-clotetrasiloxane, octyl phenyl cyclotetrasiloxane, octaphenyl-POSS, stir, be 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；
(3) 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；
(4) by above-mentioned polyisobutylene, the mixing of trimethyl hydroxyethylammonium ethylenediamine, join in the dehydrated alcohol of its weight 10-13 times, rise high-temperature and be 60-65 DEG C, insulated and stirred 10-15 minute, add the 60-70% of residue dimethyl acetylamide weight, ultrasonic 3-5 minute, obtain amide alcohol liquid；
(5) 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 amide alcohol liquid, stir, discharging, joins in the distilled water of its weight 30-40 times by product, and room temperature stands 4-5 days, filter, obtain precrosslink polyimides；
(6) by above-mentioned aluminium nitride, carborundum mixing, join in N-Methyl pyrrolidone, ultrasonic 2-3 minute, obtain aluminium nitride dispersion liquid；
(7) 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；
(8) by above-mentioned cross-linking modified polyimides, 2,4-imidazolinedione, phthalic acid dibutyl ester mix, insulated and stirred 4-7 minute at 80-90 DEG C, with remain each raw material mix, 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 resistance to acids and bases, humidity resistance, and surface strength is high, good toughness.
Detailed description of the invention
A kind of aluminium nitride strengthens heat-resistant cable material, and it is made up of the raw material of following weight parts:
2,4 imidazolinediones 0.1, tripropylene glycol methyl ether 0.1, 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, phthalic acid dibutyl ester 3, polyisobutylene 1, Zinc Pyrithione 0.8, carborundum 3, trimethyl hydroxyethylammonium ethylenediamine 0.1.
A kind of described aluminium nitride strengthens the preparation method of 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) take the 10% of above-mentioned dimethyl acetylamide weight, add above-mentioned Zinc Pyrithione, ultrasonic 2 minutes, add remaining octamethylcy-clotetrasiloxane, octyl phenyl cyclotetrasiloxane, octaphenyl POSS, stir, be 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；
(3) 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；
(4) by above-mentioned polyisobutylene, the mixing of trimethyl hydroxyethylammonium ethylenediamine, joining in the dehydrated alcohol of its weight 10 times, rising high-temperature is 60 DEG C, insulated and stirred 10 minutes, adds the 60% of residue dimethyl acetylamide weight, ultrasonic 3 minutes, obtains amide alcohol liquid；
(5) 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 amide alcohol liquid, stir, discharging, joins in the distilled water of its weight 30 times by product, and room temperature stands 4 days, filter, obtain precrosslink polyimides；
(6) by above-mentioned aluminium nitride, carborundum mixing, join in N methyl pyrrolidone, ultrasonic 2 minutes, obtain aluminium nitride dispersion liquid；
(7) 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；
(8) by above-mentioned cross-linking modified polyimides, 2,4 imidazolinediones, phthalic acid dibutyl ester mixing, insulated and stirred 4 minutes at 80 DEG C, mix with remaining each raw material, stir, be sent in screw extruder, melt extrude, cooling, pulverizing, obtain described mass.
Performance test:
Hot strength: 19.5 MPa；
Elongation at break: 354%.
Claims (2)
1. an aluminium nitride strengthens heat-resistant cable material, it is characterised in that it is made up of the raw material of following weight parts:
2, 4-imidazolinedione 0.1-0.2, tripropylene glycol methyl ether 0.1-0.3, 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, phthalic acid dibutyl ester 3-4, polyisobutylene 1-2, Zinc Pyrithione 0.8-1, carborundum 3-4, trimethyl hydroxyethylammonium ethylenediamine 0.1-0.2.
2. the preparation method of an aluminium nitride as claimed in claim 1 enhancing heat-resistant cable material, 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) take the 10-15% of above-mentioned dimethyl acetylamide weight, add above-mentioned Zinc Pyrithione, ultrasonic 2-3 minute, add remaining octamethylcy-clotetrasiloxane, octyl phenyl cyclotetrasiloxane, octaphenyl-POSS, stir, be 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；
(3) 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；
(4) by above-mentioned polyisobutylene, the mixing of trimethyl hydroxyethylammonium ethylenediamine, join in the dehydrated alcohol of its weight 10-13 times, rise high-temperature and be 60-65 DEG C, insulated and stirred 10-15 minute, add the 60-70% of residue dimethyl acetylamide weight, ultrasonic 3-5 minute, obtain amide alcohol liquid；
(5) 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 amide alcohol liquid, stir, discharging, joins in the distilled water of its weight 30-40 times by product, and room temperature stands 4-5 days, filter, obtain precrosslink polyimides；
(6) by above-mentioned aluminium nitride, carborundum mixing, join in N-Methyl pyrrolidone, ultrasonic 2-3 minute, obtain aluminium nitride dispersion liquid；
(7) 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；
(8) by above-mentioned cross-linking modified polyimides, 2,4-imidazolinedione, phthalic acid dibutyl ester mix, insulated and stirred 4-7 minute at 80-90 DEG C, with remain each raw material mix, stir, be sent in screw extruder, melt extrude, cooling, pulverizing, obtain described mass.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106566146A (en) * | 2016-10-19 | 2017-04-19 | 安徽吉思特智能装备有限公司 | Hydrophobic high dielectric material and preparation method thereof |
| CN108329552A (en) * | 2018-02-24 | 2018-07-27 | 四会市启德信息咨询服务有限公司 | A kind of corrosion-resistant high electrolyte release rate battery separator material |
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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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| Publication number | Priority date | Publication date | Assignee | Title |
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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 |
Non-Patent Citations (2)
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| 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》 * |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106566146A (en) * | 2016-10-19 | 2017-04-19 | 安徽吉思特智能装备有限公司 | Hydrophobic high dielectric material and preparation method thereof |
| CN108329552A (en) * | 2018-02-24 | 2018-07-27 | 四会市启德信息咨询服务有限公司 | A kind of corrosion-resistant high electrolyte release rate battery separator material |
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