CN105924743A - Aluminum sol modified heatproof optical cable material and preparation method thereof - Google Patents
Aluminum sol modified heatproof optical cable material and preparation method thereof Download PDFInfo
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- CN105924743A CN105924743A CN201610457074.7A CN201610457074A CN105924743A CN 105924743 A CN105924743 A CN 105924743A CN 201610457074 A CN201610457074 A CN 201610457074A CN 105924743 A CN105924743 A CN 105924743A
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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
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- 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 an aluminum sol modified heatproof optical cable material. The aluminum sol modified heatproof optical cable material is prepared from the following raw materials in parts by weight: 3-5 parts of aluminium isopropoxide, 1-2 parts of ammonium molybdate, 5-7 parts of octamethylcyclotetrasiloxane, 2-3 parts of octaphenyl-POSS, 0.01-0.02 part of tetramethylammonium hydroxide, 300-400 parts of dimethylacetamide, 1-3 parts of octaphenylcyclotetrasiloxane, 37-40 parts of 4,4'-diaminodiphenyl ether, 2-4 parts of 20-25% ammonia, 46-50 parts of pyromellitic acid dianhydride, 70-80 parts of N-methyl-2-pyrrolidone, 3-4 parts of aluminum nitride, 100-110 parts of high-density polyethylene, 0.1-0.2 part of diaminodiphenyl ether, 0.7-1 part of didecyldimethylammonium bromide, 3-4 parts of terpilenol, 0.4-1 part of hydroxyquinoline, and 4-6 parts of 2-ethylhexyl epoxystearate. According to the aluminum sol modified heatproof optical cable material, the dispersibility of fillers in a polymer is effectively improved, and meanwhile, the surface resistance of a finished-product material is improved.
Description
Technical field
The present invention relates to mass technical field, particularly relate to a kind of Alumina gel modified heat resistant mass 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 Ultramicro-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 heat resistance, 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 Alumina gel modified heat resistant mass and preparation method thereof.
The present invention is achieved by the following technical solutions:
A kind of Alumina gel modified heat resistant mass, it is made up of the raw material of following weight parts:
Aluminium isopropoxide 3-5, ammonium molybdate 1-2, octamethylcy-clotetrasiloxane 5-7, octaphenyl-POSS2-3, TMAH 0.01-0.02, dimethylacetylamide 300-400, octyl phenyl cyclotetrasiloxane 1-3,4, the ammoniacal liquor 2-4 of 4'-diaminodiphenyl ether 37-40,20-25%, pyromellitic acid anhydride 46-50,1-METHYLPYRROLIDONE 70-80, aluminium nitride 3-4, high density polyethylene (HDPE) 100-110, diaminodiphenyl ether 0.1-0.2, double decyl dimethyl ammonium bromide 0.7-1, terpinol 3-4,8-hydroxyquinoline 0.4-1, octyl epoxy stearate 4-6.
The preparation method of a kind of described Alumina gel modified heat resistant mass, comprises the following steps:
(1) taking the 10-15% of above-mentioned octamethylcy-clotetrasiloxane weight, mix with TMAH, be passed through nitrogen, insulation reaction 2-3 hour at 90-95 DEG C, slowly reducing temperature is normal temperature, obtains alkaline-sol;
(2) above-mentioned 8-hydroxyquinoline is joined in its weight 27-30 times, 30-35% ethanol solution, rise high-temperature and be 50-60 DEG C, add above-mentioned aluminium isopropoxide, insulated and stirred 10-20 minute, adds the 10-12% of above-mentioned alkaline-sol weight, rises high-temperature and is 70-80 DEG C, insulated and stirred 17-20 minute, adding ammonium molybdate, stirring, to normal temperature, obtains modified aluminium colloidal sol;
(3) take the 10-15% of above-mentioned dimethylacetylamide weight, add remaining octamethylcy-clotetrasiloxane, octyl phenyl cyclotetrasiloxane, octaphenyl-POSS, stir, it is passed through nitrogen, add remaining 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 ammoniacal liquor 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) by above-mentioned ammonium molybdate, the mixing of double decyl dimethyl ammonium bromide, join in the distilled water of compound weight 20-30 times, stir, obtain aqueous dispersions;
(6) by above-mentioned refined phenylate, pyromellitic acid anhydride, cross linking polysiloxane mixing, add remaining dimethylacetylamide, stir, send in ice-water bath, be passed through nitrogen, stirring reaction 2-3 hour, discharging, joins product in above-mentioned aqueous dispersions, and normal temperature stands 4-5 days, filter, obtain precrosslink polyimides;
(7) above-mentioned aluminium nitride is joined in 1-METHYLPYRROLIDONE, 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, add above-mentioned modified aluminium colloidal sol, stir, filter, it will be vacuum dried 3-5 hour at being deposited in 76-80 DEG C, wear into fine powder, send in the vacuum drying chamber of 250-260 DEG C, heat 6-7 hour, discharging cools down, and obtains cross-linking modified polyimides;
(9) above-mentioned cross-linking modified polyimides is mixed with remaining each raw material, stir, be sent in screw extruder, melt extrude, cooling, abrasive dust, 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 1-METHYLPYRROLIDONE 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 particle, 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 endurance 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 present invention uses aluminium isopropoxide to be presoma, and the Alumina gel obtained can effectively improve filler dispersiveness in the polymer, improves the surface resistive of finished-product material simultaneously.
Detailed description of the invention
A kind of Alumina gel modified heat resistant mass, it is made up of the raw material of following weight parts:
Aluminium isopropoxide 3, ammonium molybdate 1, octamethylcy-clotetrasiloxane 5, octaphenyl POSS2, TMAH 0.01, dimethylacetylamide 300, octyl phenyl cyclotetrasiloxane 1,4, the ammoniacal liquor 2 of 4' diaminodiphenyl ether 37,20%, pyromellitic acid anhydride 46, N methyl pyrrolidone 70, aluminium nitride 3, high density polyethylene (HDPE) 100, diaminodiphenyl ether 0.1, double decyl dimethyl ammonium bromide 0.7, terpinol 3,8 oxyquinoline 0.4, octyl epoxy stearate 4.
The preparation method of a kind of described Alumina gel modified heat resistant mass, comprises the following steps:
(1) taking the 10% of above-mentioned octamethylcy-clotetrasiloxane weight, mix with TMAH, be passed through nitrogen, insulation reaction 2 hours at 90 DEG C, slowly reducing temperature is normal temperature, obtains alkaline-sol;
(2) above-mentioned 8 oxyquinolines are joined in its weight 27 times, the ethanol solution of 30%, rising high-temperature is 50 DEG C, add above-mentioned aluminium isopropoxide, insulated and stirred 10 minutes, adds the 10% of above-mentioned alkaline-sol weight, and rising high-temperature is 70 DEG C, insulated and stirred 17 minutes, adding ammonium molybdate, stirring, to normal temperature, obtains modified aluminium colloidal sol;
(3) take the 10% of above-mentioned dimethylacetylamide weight, add remaining octamethylcy-clotetrasiloxane, octyl phenyl cyclotetrasiloxane, octaphenyl POSS, stir, it is passed through nitrogen, add remaining 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 ammoniacal liquor 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) by above-mentioned ammonium molybdate, the mixing of double decyl dimethyl ammonium bromide, join in the distilled water of compound weight 20 times, stir, obtain aqueous dispersions;
(6) by above-mentioned refined phenylate, pyromellitic acid anhydride, cross linking polysiloxane mixing, add remaining dimethylacetylamide, stir, send in ice-water bath, be passed through nitrogen, stirring reaction 2 hours, discharging, joins product in above-mentioned aqueous dispersions, and normal 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, add above-mentioned modified aluminium colloidal sol, stir, filter, vacuum drying 3 hours will be deposited at 76 DEG C, wear into fine powder, send in the vacuum drying chamber of 250 DEG C, heat 6 hours, discharging cools down, and obtains cross-linking modified polyimides;
(9) above-mentioned cross-linking modified polyimides is mixed with remaining each raw material, stir, be sent in screw extruder, melt extrude, cooling, abrasive dust, obtain described mass.
Performance test:
Hot strength: 19.9MPa;
Elongation at break: 351%.
Claims (2)
1. an Alumina gel modified heat resistant mass, it is characterised in that it is made up of the raw material of following weight parts:
Aluminium isopropoxide 3-5, ammonium molybdate 1-2, octamethylcy-clotetrasiloxane 5-7, octaphenyl-POSS2-3, TMAH 0.01-0.02, dimethylacetylamide 300-400, octyl phenyl cyclotetrasiloxane 1-3,4, the ammoniacal liquor 2-4 of 4'-diaminodiphenyl ether 37-40,20-25%, pyromellitic acid anhydride 46-50,1-METHYLPYRROLIDONE 70-80, aluminium nitride 3-4, high density polyethylene (HDPE) 100-110, diaminodiphenyl ether 0.1-0.2, double decyl dimethyl ammonium bromide 0.7-1, terpinol 3-4,8-hydroxyquinoline 0.4-1, octyl epoxy stearate 4-6.
2. the preparation method of an Alumina gel modified heat resistant mass 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 TMAH, be passed through nitrogen, insulation reaction 2-3 hour at 90-95 DEG C, slowly reducing temperature is normal temperature, obtains alkaline-sol;
(2) above-mentioned 8-hydroxyquinoline is joined in its weight 27-30 times, 30-35% ethanol solution, rise high-temperature and be 50-60 DEG C, add above-mentioned aluminium isopropoxide, insulated and stirred 10-20 minute, adds the 10-12% of above-mentioned alkaline-sol weight, rises high-temperature and is 70-80 DEG C, insulated and stirred 17-20 minute, adding ammonium molybdate, stirring, to normal temperature, obtains modified aluminium colloidal sol;
(3) take the 10-15% of above-mentioned dimethylacetylamide weight, add remaining octamethylcy-clotetrasiloxane, octyl phenyl cyclotetrasiloxane, octaphenyl-POSS, stir, it is passed through nitrogen, add remaining 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 ammoniacal liquor 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) by above-mentioned ammonium molybdate, the mixing of double decyl dimethyl ammonium bromide, join in the distilled water of compound weight 20-30 times, stir, obtain aqueous dispersions;
(6) by above-mentioned refined phenylate, pyromellitic acid anhydride, cross linking polysiloxane mixing, add remaining dimethylacetylamide, stir, send in ice-water bath, be passed through nitrogen, stirring reaction 2-3 hour, discharging, joins product in above-mentioned aqueous dispersions, and normal temperature stands 4-5 days, filter, obtain precrosslink polyimides;
(7) above-mentioned aluminium nitride is joined in 1-METHYLPYRROLIDONE, 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, add above-mentioned modified aluminium colloidal sol, stir, filter, it will be vacuum dried 3-5 hour at being deposited in 76-80 DEG C, wear into fine powder, send in the vacuum drying chamber of 250-260 DEG C, heat 6-7 hour, discharging cools down, and obtains cross-linking modified polyimides;
(9) above-mentioned cross-linking modified polyimides is mixed with remaining each raw material, stir, be sent in screw extruder, melt extrude, cooling, abrasive dust, obtain described mass.
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Cited By (3)
Publication number | Priority date | Publication date | Assignee | Title |
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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 |
CN106565918A (en) * | 2016-10-26 | 2017-04-19 | 章功国 | Silane modified polymer coated dielectric material and preparation method thereof |
CN106675389A (en) * | 2016-12-16 | 2017-05-17 | 安徽荣玖智能装备科技有限公司 | Aluminum sol composite polyimide powder paint and preparation method thereof |
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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 (3)
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 |
CN106565918A (en) * | 2016-10-26 | 2017-04-19 | 章功国 | Silane modified polymer coated dielectric material and preparation method thereof |
CN106675389A (en) * | 2016-12-16 | 2017-05-17 | 安徽荣玖智能装备科技有限公司 | Aluminum sol composite polyimide powder paint and preparation method thereof |
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Application publication date: 20160907 |