CN109233710A - Insulating material with high glass transition temperature and high-temperature cohesiveness and preparation method thereof - Google Patents
Insulating material with high glass transition temperature and high-temperature cohesiveness and preparation method thereof Download PDFInfo
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- CN109233710A CN109233710A CN201810662025.6A CN201810662025A CN109233710A CN 109233710 A CN109233710 A CN 109233710A CN 201810662025 A CN201810662025 A CN 201810662025A CN 109233710 A CN109233710 A CN 109233710A
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- 238000002360 preparation method Methods 0.000 title claims abstract description 29
- 239000011810 insulating material Substances 0.000 title claims abstract description 25
- 230000009477 glass transition Effects 0.000 title claims abstract description 21
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims abstract description 28
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 25
- 239000000203 mixture Substances 0.000 claims abstract description 25
- 229910052710 silicon Inorganic materials 0.000 claims abstract description 25
- 239000010703 silicon Substances 0.000 claims abstract description 25
- 239000002270 dispersing agent Substances 0.000 claims abstract description 21
- 239000003822 epoxy resin Substances 0.000 claims abstract description 20
- 229920000647 polyepoxide Polymers 0.000 claims abstract description 20
- 239000011342 resin composition Substances 0.000 claims abstract description 18
- 239000012745 toughening agent Substances 0.000 claims abstract description 11
- 229920002635 polyurethane Polymers 0.000 claims abstract description 10
- 239000004814 polyurethane Substances 0.000 claims abstract description 10
- KXGFMDJXCMQABM-UHFFFAOYSA-N 2-methoxy-6-methylphenol Chemical compound [CH]OC1=CC=CC([CH])=C1O KXGFMDJXCMQABM-UHFFFAOYSA-N 0.000 claims abstract description 9
- 229920001568 phenolic resin Polymers 0.000 claims abstract description 9
- 239000005011 phenolic resin Substances 0.000 claims abstract description 9
- 229920005989 resin Polymers 0.000 claims abstract description 9
- 239000011347 resin Substances 0.000 claims abstract description 9
- 238000012986 modification Methods 0.000 claims abstract description 6
- 230000004048 modification Effects 0.000 claims abstract description 6
- 238000003756 stirring Methods 0.000 claims description 24
- 229920002134 Carboxymethyl cellulose Polymers 0.000 claims description 18
- 239000001768 carboxy methyl cellulose Substances 0.000 claims description 18
- 235000010948 carboxy methyl cellulose Nutrition 0.000 claims description 18
- 239000008112 carboxymethyl-cellulose Substances 0.000 claims description 18
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 claims description 16
- FEWJPZIEWOKRBE-UHFFFAOYSA-N Tartaric acid Natural products [H+].[H+].[O-]C(=O)C(O)C(O)C([O-])=O FEWJPZIEWOKRBE-UHFFFAOYSA-N 0.000 claims description 15
- 239000011975 tartaric acid Substances 0.000 claims description 15
- 235000002906 tartaric acid Nutrition 0.000 claims description 15
- 238000000034 method Methods 0.000 claims description 14
- 238000006243 chemical reaction Methods 0.000 claims description 12
- 238000010792 warming Methods 0.000 claims description 11
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 10
- 229960000935 dehydrated alcohol Drugs 0.000 claims description 10
- 239000004519 grease Substances 0.000 claims description 10
- BDAGIHXWWSANSR-UHFFFAOYSA-N methanoic acid Natural products OC=O BDAGIHXWWSANSR-UHFFFAOYSA-N 0.000 claims description 10
- 238000010992 reflux Methods 0.000 claims description 10
- 230000008569 process Effects 0.000 claims description 9
- VLDPXPPHXDGHEW-UHFFFAOYSA-N 1-chloro-2-dichlorophosphoryloxybenzene Chemical compound ClC1=CC=CC=C1OP(Cl)(Cl)=O VLDPXPPHXDGHEW-UHFFFAOYSA-N 0.000 claims description 8
- 229920002565 Polyethylene Glycol 400 Polymers 0.000 claims description 8
- JLFNLZLINWHATN-UHFFFAOYSA-N pentaethylene glycol Chemical compound OCCOCCOCCOCCOCCO JLFNLZLINWHATN-UHFFFAOYSA-N 0.000 claims description 8
- 239000011780 sodium chloride Substances 0.000 claims description 8
- KTWOOEGAPBSYNW-UHFFFAOYSA-N ferrocene Chemical compound [Fe+2].C=1C=C[CH-]C=1.C=1C=C[CH-]C=1 KTWOOEGAPBSYNW-UHFFFAOYSA-N 0.000 claims description 7
- 238000004519 manufacturing process Methods 0.000 claims description 7
- 238000007664 blowing Methods 0.000 claims description 6
- 239000006185 dispersion Substances 0.000 claims description 6
- 238000010438 heat treatment Methods 0.000 claims description 6
- 238000007711 solidification Methods 0.000 claims description 6
- 230000008023 solidification Effects 0.000 claims description 6
- 238000003860 storage Methods 0.000 claims description 6
- OSWFIVFLDKOXQC-UHFFFAOYSA-N 4-(3-methoxyphenyl)aniline Chemical compound COC1=CC=CC(C=2C=CC(N)=CC=2)=C1 OSWFIVFLDKOXQC-UHFFFAOYSA-N 0.000 claims description 5
- 150000001875 compounds Chemical class 0.000 claims description 5
- 238000002425 crystallisation Methods 0.000 claims description 5
- 230000008025 crystallization Effects 0.000 claims description 5
- 230000008020 evaporation Effects 0.000 claims description 5
- 238000001704 evaporation Methods 0.000 claims description 5
- 238000001914 filtration Methods 0.000 claims description 5
- 235000019253 formic acid Nutrition 0.000 claims description 5
- 238000007789 sealing Methods 0.000 claims description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 5
- FEWJPZIEWOKRBE-JCYAYHJZSA-N Dextrotartaric acid Chemical compound OC(=O)[C@H](O)[C@@H](O)C(O)=O FEWJPZIEWOKRBE-JCYAYHJZSA-N 0.000 claims description 4
- 239000006087 Silane Coupling Agent Substances 0.000 claims description 4
- 239000002253 acid Substances 0.000 claims description 3
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims 1
- KDFQYGBJUYYWDJ-UHFFFAOYSA-N azane;sodium Chemical compound N.[Na] KDFQYGBJUYYWDJ-UHFFFAOYSA-N 0.000 claims 1
- 235000009508 confectionery Nutrition 0.000 claims 1
- 238000001035 drying Methods 0.000 claims 1
- 229910052760 oxygen Inorganic materials 0.000 claims 1
- 239000001301 oxygen Substances 0.000 claims 1
- 239000011863 silicon-based powder Substances 0.000 abstract description 3
- 229910052751 metal Inorganic materials 0.000 abstract description 2
- 239000002184 metal Substances 0.000 abstract description 2
- 230000000704 physical effect Effects 0.000 abstract description 2
- 239000002131 composite material Substances 0.000 abstract 1
- 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 abstract 1
- 239000004593 Epoxy Substances 0.000 description 11
- 230000008859 change Effects 0.000 description 6
- 229920001296 polysiloxane Polymers 0.000 description 5
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 description 4
- 150000001412 amines Chemical class 0.000 description 4
- 125000001797 benzyl group Chemical group [H]C1=C([H])C([H])=C(C([H])=C1[H])C([H])([H])* 0.000 description 4
- 239000008367 deionised water Substances 0.000 description 4
- 229910021641 deionized water Inorganic materials 0.000 description 4
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 description 4
- 239000000463 material Substances 0.000 description 4
- 229910000077 silane Inorganic materials 0.000 description 4
- NIXOWILDQLNWCW-UHFFFAOYSA-M acrylate group Chemical group C(C=C)(=O)[O-] NIXOWILDQLNWCW-UHFFFAOYSA-M 0.000 description 3
- 230000006872 improvement Effects 0.000 description 3
- 239000002994 raw material Substances 0.000 description 3
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 2
- 150000008064 anhydrides Chemical class 0.000 description 2
- 238000005452 bending Methods 0.000 description 2
- 150000002632 lipids Chemical class 0.000 description 2
- 239000010754 BS 2869 Class F Substances 0.000 description 1
- 230000001070 adhesive effect Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 125000000058 cyclopentadienyl group Chemical group C1(=CC=CC1)* 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- XXBDWLFCJWSEKW-UHFFFAOYSA-N dimethylbenzylamine Chemical compound CN(C)CC1=CC=CC=C1 XXBDWLFCJWSEKW-UHFFFAOYSA-N 0.000 description 1
- 238000004945 emulsification Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000032050 esterification Effects 0.000 description 1
- 238000005886 esterification reaction Methods 0.000 description 1
- 150000002460 imidazoles Chemical class 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 238000000465 moulding Methods 0.000 description 1
- 230000003381 solubilizing effect Effects 0.000 description 1
- 239000004575 stone Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J163/00—Adhesives based on epoxy resins; Adhesives based on derivatives of epoxy resins
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
- C09J11/02—Non-macromolecular additives
- C09J11/04—Non-macromolecular additives inorganic
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
- C09J11/02—Non-macromolecular additives
- C09J11/06—Non-macromolecular additives organic
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
- C09J11/08—Macromolecular additives
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/02—Elements
- C08K2003/023—Silicon
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/02—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group
- C08L2205/025—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group containing two or more polymers of the same hierarchy C08L, and differing only in parameters such as density, comonomer content, molecular weight, structure
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend
- C08L2205/035—Polymer mixtures characterised by other features containing three or more polymers in a blend containing four or more polymers in a blend
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Compositions Of Macromolecular Compounds (AREA)
Abstract
The invention discloses an insulating material with high glass transition temperature and high-temperature cohesiveness and a preparation method thereof, and relates to the technical field of insulating materials. The insulating material of the present invention is obtained by reacting a resin composition and a curing agent composition, the resin composition comprising: four-functional group epoxy resin, organic silicon epoxy resin, phenolic resin, polyurethane modified epoxy resin and a dispersing agent; the curing agent composition comprises: pyromellitic anhydride, a toughening agent and a composite accelerator. The invention also carries out modification treatment on the metal silicon powder, enhances the affinity of the silicon powder to resin, and improves the physical property and the glass transition temperature of the insulating material.
Description
Technical field:
The present invention relates to insulating materials technical fields, and in particular to one kind has high glass-transition temperature, high temperature bond
The insulating materials and preparation method thereof of property.
Background technique:
The glass transition temperature of traditional epoxy anhydride system insulating part is generally all within 130 degree, although possessing higher
Glass transition temperature, but increasingly developed electric utility just cannot obviously be met the requirements.According to the needs of the market, we
The formula and technique of traditional epoxy anhydride system insulating part are improved, it is high, high to provide a kind of glass transition temperature
The excellent insulating materials of warm adhesive property, glass transition temperature can achieve 160 degree or more, can satisfy existing electric power completely
Growth requirement.
Summary of the invention:
It is exhausted technical problem to be solved by the present invention lies in providing that a kind of glass transition temperature is high, high temperature bond performance is excellent
Edge material.
The following technical solution is employed for the technical problems to be solved by the invention to realize: one kind having high glass transition
The insulating materials of temperature, elevated temperature cohesiveness is reacted to obtain by modified resin composition with curing agent composition.
The modified resin composition includes the raw material of following parts by weight:
The curing agent composition includes the raw material of following parts by weight:
89.4 parts of pyromellitic dianhydride
10 parts of toughener
0.6 part of compound accelerant.
The four-functional group epoxy resin is selected from the graceful four-functional group epoxy resin of Hensel.
The organosilicon epoxy resin is selected from the graceful machine epoxy silicone of Hensel.
The molecular weight of the phenolic resin is 5000-2 ten thousand.
The polyurethane modified epoxy resin is selected from polyurethane modified epoxy resin SL3451.
The dispersing agent is carboxymethyl cellulose/tartaric acid, preparation method are as follows: carboxymethyl cellulose is added in right amount
Deionized water in, stirring at normal temperature is to being completely dissolved；Adjusting the pH of solution with 10% acetum is 5-6, adds two cyclopentadienyls
Iron and tartaric acid, are warming up to 70-80 DEG C of stirring 2-3h, and grease occurs in reaction system；It is cooled to 30-40 DEG C, sodium chloride is added
0.5-1h is stirred with NaGC；It is cooled to room temperature, isolates grease, evaporation, crystallization obtain carboxymethyl cellulose/wine
Stone acid.
The carboxymethyl cellulose, ferrocene, tartaric acid, sodium chloride, NaGC mass ratio be 30-40:1:20-
30:2:2.
The mechanism of above-mentioned reaction is esterification, and carboxymethyl cellulose and tartaric acid are in acid condition to urge with ferrocene
Agent has synthesized carboxymethyl cellulose/tartaric acid, using the saltouing of sodium chloride and NaGC, is modified, is dispersed
Agent.The dispersing agent has good intermiscibility for lipid material and resin, simultaneously because the change of structure, so that synthetic dispersing agent
Emulsification, solubilizing effect will be much higher than carboxymethyl cellulose.
The preferred Tao Shi chemical industry toughener F-10 of toughener.
The compound accelerant is selected from one of benzyl dimethylamine, imidazoles or a variety of.
A kind of preparation method with high glass-transition temperature, the insulating materials of elevated temperature cohesiveness, comprising the following steps:
(1) preparation of modified resin composition: four-functional group epoxy resin is added in high speed dispersion storage tank, is preheated to 80
℃；It is subsequently added into organosilicon epoxy resin, phenolic resin, polyurethane modified epoxy resin, 400-600r/min revolving speed stirs mixed
1h is closed, is cooled to 64-65 DEG C of addition dispersing agent, 500r/min revolving speed is stirred 1h, then blowing；
(2) preparation of curing agent composition: pyromellitic dianhydride is added in reaction kettle, and stirring is warming up to 105 DEG C, then
Toughener is added, after 40-60r/min revolving speed insulated and stirred 3h, is cooled to 70-75 DEG C, compound accelerant, insulated and stirred is added
20-30min；
(3) heating cure forms: by the composition of modified resin composition, curing agent and metallic silicon power according to mass ratio
100:60:300 is mixed evenly, and the production of mutual inductor is carried out by way of vacuum pouring, is solidified using 80 DEG C
2h, 110 DEG C solidify 2h, 130 DEG C of curing process for solidifying 6-8h are solidified.
The metallic silicon power passes through modification, method of modifying are as follows: metallic silicon power is dispersed in dehydrated alcohol, is soaked
10-15min is steeped, pH value of solution is adjusted with formic acid and PEG400 is then added to 5-6, and be heated to reflux state insulated and stirred 15-
30min adds silane coupling agent, continues insulated and stirred 0.5-2h at reflux, cooled to room temperature, gained mixing
Object is transferred to sealing and standing 2-6h in -5 DEG C of environment, filtering, and gained filter residue is sent into vacuum drier after being washed with dehydrated alcohol and is done
It is dry.
The metallic silicon power, PEG400, silane coupling agent mass ratio be 10-15:1-5:1-5.
The granularity of the metallic silicon power is 40-100 mesh.
The beneficial effects of the present invention are:
(1) four kinds of resins and dispersing agent are mixed composition modified resin composition by the present invention in proportion, and composition is cured
After agent curing molding, glass transition temperature and elevated temperature cohesiveness with higher；
(2) using carboxymethyl cellulose, tartaric acid as the dispersing agent of raw material, the resin of different component can be uniformly mixed, shape
At the high resin system of a dispersibility, while improving the elevated temperature cohesiveness of resin system；In the curing process, dispersing agent energy
It assists curing agent composition to reduce curing time, improve solidification intensity, has obviously to the physical mechanical property of final insulating materials
Improvement；
(3) metallic silicon power reduces the hardness of itself, avoids metallic silicon power after PEG400, silane coupler modified
The defect for causing granularity to decline because matter is hard frangible in whipping process；The addition of metallic silicon power improves resin stretched, bending
Etc. physical properties；Modified metal silicon powder is significantly improved to the compatibility of lipid material, while metallic silicon power can improve
The glass transition temperature of material meets the needs of F, H class F insulating material F；
(4) the simple and environmentally-friendly suitable industrialized production of process flow.
Specific embodiment:
In order to be easy to understand the technical means, the creative features, the aims and the efficiencies achieved by the present invention, tie below
Specific embodiment is closed, the present invention is further explained.
Embodiment 1
The preparation of dispersing agent: being added to 30g carboxymethyl cellulose in suitable deionized water, stirring at normal temperature to completely it is molten
Solution；Adjusting the pH of solution with 10% acetum is 5-6, adds 1g ferrocene and 20g tartaric acid, is warming up to 70 DEG C of stirrings
There is grease in 2h, reaction system；35 DEG C are cooled to, 2g sodium chloride is added and 2g NaGC stirs 0.5h；It is cooled to room
Temperature, isolates grease, and evaporation, crystallization obtain carboxymethyl cellulose/tartaric acid.
The preparation of insulating materials:
(1) high speed dispersion storage tank the preparation of modified resin composition: is added in the graceful four-functional group epoxy resin of 70g Hensel
In, it is preheated to 80 DEG C；It has been subsequently added into the graceful machine epoxy silicone of 10g Hensel, 10g phenolic resin, 10g polyurethane modified epoxy tree
Rouge SL3451,400r/min revolving speed is stirred 1h, is cooled to 64-65 DEG C of addition 8g dispersing agent, and the stirring of 500r/min revolving speed is mixed
1h is closed, then blowing；
(2) preparation of curing agent composition: 89.4g pyromellitic dianhydride is added in reaction kettle, and stirring is warming up to 105
DEG C, 10g toughener F-10 is added, after 40r/min revolving speed insulated and stirred 3h, 70 DEG C is cooled to, 0.6g benzyl diformazan is added
Amine, insulated and stirred 20min；
(3) heating cure forms: by 100g modified resin composition, 60g curing agent composition and 300g metallic silicon power
It is mixed evenly, the production of mutual inductor is carried out by way of vacuum pouring, consolidated using 80 DEG C of solidification 2h, 110 DEG C
Change 2h, 130 DEG C of curing process for solidifying 6h are solidified.
The modification of metallic silicon power: 10g metallic silicon power is dispersed in dehydrated alcohol, is impregnated 10min, is adjusted with formic acid
Then 2g PEG400 is added to 5-6 in pH value of solution, and be heated to reflux state insulated and stirred 20min, and it is silane coupled to add 2g
Agent, insulated and stirred 1h, cooled to room temperature, gained mixture are transferred to sealing and standing in -5 DEG C of environment at reflux for continuation
3h, filtering, gained filter residue are sent into dry in vacuum drier after being washed with dehydrated alcohol.
Embodiment 2
The preparation of dispersing agent: being added to 35g carboxymethyl cellulose in suitable deionized water, stirring at normal temperature to completely it is molten
Solution；Adjusting the pH of solution with 10% acetum is 5-6, adds 1g ferrocene and 22g tartaric acid, is warming up to 70 DEG C of stirrings
There is grease in 2h, reaction system；35 DEG C are cooled to, 2g sodium chloride is added and 2g NaGC stirs 0.5h；It is cooled to room
Temperature, isolates grease, and evaporation, crystallization obtain carboxymethyl cellulose/tartaric acid.
The preparation of insulating materials:
(1) high speed dispersion storage tank the preparation of modified resin composition: is added in the graceful four-functional group epoxy resin of 70g Hensel
In, it is preheated to 80 DEG C；It has been subsequently added into the graceful machine epoxy silicone of 10g Hensel, 10g phenolic resin, 10g polyurethane modified epoxy tree
Rouge SL3451,400r/min revolving speed is stirred 1h, is cooled to 64-65 DEG C of addition 8g dispersing agent, and the stirring of 500r/min revolving speed is mixed
1h is closed, then blowing；
(2) preparation of curing agent composition: 89.4g pyromellitic dianhydride is added in reaction kettle, and stirring is warming up to 105
DEG C, 10g toughener F-10 is added, after 40r/min revolving speed insulated and stirred 3h, 70 DEG C is cooled to, 0.6g benzyl diformazan is added
Amine, insulated and stirred 20min；
(3) heating cure forms: by 100g modified resin composition, 60g curing agent composition and 300g metallic silicon power
It is mixed evenly, the production of mutual inductor is carried out by way of vacuum pouring, consolidated using 80 DEG C of solidification 2h, 110 DEG C
Change 2h, 130 DEG C of curing process for solidifying 6h are solidified.
The modification of metallic silicon power: 10g metallic silicon power is dispersed in dehydrated alcohol, is impregnated 10min, is adjusted with formic acid
Then 2g PEG400 is added to 5-6 in pH value of solution, and be heated to reflux state insulated and stirred 20min, and it is silane coupled to add 3g
Agent, insulated and stirred 1h, cooled to room temperature, gained mixture are transferred to sealing and standing in -5 DEG C of environment at reflux for continuation
3h, filtering, gained filter residue are sent into dry in vacuum drier after being washed with dehydrated alcohol.
Reference examples 1
Dispersing agent is selected from acrylate dispersant, molecular weight 1000-5000.
The preparation of insulating materials:
(1) high speed dispersion storage tank the preparation of modified resin composition: is added in the graceful four-functional group epoxy resin of 70g Hensel
In, it is preheated to 80 DEG C；It has been subsequently added into the graceful machine epoxy silicone of 10g Hensel, 10g phenolic resin, 10g polyurethane modified epoxy tree
Rouge SL3451,400r/min revolving speed is stirred 1h, is cooled to 64-65 DEG C of addition 8g acrylate dispersant, and 500r/min turns
Speed is stirred 1h, then blowing；
(2) preparation of curing agent composition: 89.4g pyromellitic dianhydride is added in reaction kettle, and stirring is warming up to 105
DEG C, 10g toughener F-10 is added, after 40r/min revolving speed insulated and stirred 3h, 70 DEG C is cooled to, 0.6g benzyl diformazan is added
Amine, insulated and stirred 20min；
(3) heating cure forms: by 100g modified resin composition, 60g curing agent composition and 300g metallic silicon power
It is mixed evenly, the production of mutual inductor is carried out by way of vacuum pouring, consolidated using 80 DEG C of solidification 2h, 110 DEG C
Change 2h, 130 DEG C of curing process for solidifying 6h are solidified.
The modification of metallic silicon power: 10g metallic silicon power is dispersed in dehydrated alcohol, is impregnated 10min, is adjusted with formic acid
Then 2g PEG400 is added to 5-6 in pH value of solution, and be heated to reflux state insulated and stirred 20min, and it is silane coupled to add 3g
Agent, insulated and stirred 1h, cooled to room temperature, gained mixture are transferred to sealing and standing in -5 DEG C of environment at reflux for continuation
3h, filtering, gained filter residue are sent into dry in vacuum drier after being washed with dehydrated alcohol.
Reference examples 2
The preparation of dispersing agent: being added to 35g carboxymethyl cellulose in suitable deionized water, stirring at normal temperature to completely it is molten
Solution；Adjusting the pH of solution with 10% acetum is 5-6, adds 1g ferrocene and 22g tartaric acid, is warming up to 70 DEG C of stirrings
There is grease in 2h, reaction system；35 DEG C are cooled to, 2g sodium chloride is added and 2g NaGC stirs 0.5h；It is cooled to room
Temperature, isolates grease, and evaporation, crystallization obtain carboxymethyl cellulose/tartaric acid.
The preparation of insulating materials:
(1) high speed dispersion storage tank the preparation of modified resin composition: is added in the graceful four-functional group epoxy resin of 70g Hensel
In, it is preheated to 80 DEG C；It has been subsequently added into the graceful machine epoxy silicone of 10g Hensel, 10g phenolic resin, 10g polyurethane modified epoxy tree
Rouge SL3451,400r/min revolving speed is stirred 1h, is cooled to 64-65 DEG C of addition 8g dispersing agent, and the stirring of 500r/min revolving speed is mixed
1h is closed, then blowing；
(2) preparation of curing agent composition: 89.4g pyromellitic dianhydride is added in reaction kettle, and stirring is warming up to 105
DEG C, 10g toughener F-10 is added, after 40r/min revolving speed insulated and stirred 3h, 70 DEG C is cooled to, 0.6g benzyl diformazan is added
Amine, insulated and stirred 20min；
(3) heating cure forms: by 100g modified resin composition, 60g curing agent composition and 300g metallic silicon power
It is mixed evenly, the production of mutual inductor is carried out by way of vacuum pouring, consolidated using 80 DEG C of solidification 2h, 110 DEG C
Change 2h, 130 DEG C of curing process for solidifying 6h are solidified.
Embodiment 3
Based on embodiment 2, setting uses the reference examples 1 of acrylate dispersant, is not modified to metallic silicon power
Reference examples 2.
Be utilized respectively embodiment 1-2, reference examples 1-2 prepares insulating materials, and be used for performance and tested, as a result such as
Shown in table 1.
The service performance of 1 insulating materials of table
Test method: tensile strength ASTM D638；Bending strength ASTM D790；Glass transition temperature DCS.
The above shows and describes the basic principles and main features of the present invention and the advantages of the present invention.The technology of the industry
Personnel are it should be appreciated that the present invention is not limited to the above embodiments, and the above embodiments and description only describe this
The principle of invention, without departing from the spirit and scope of the present invention, various changes and improvements may be made to the invention, these changes
Change and improvement all fall within the protetion scope of the claimed invention.The claimed scope of the invention by appended claims and its
Equivalent thereof.
Claims (6)
1. a kind of insulating materials with high glass-transition temperature, elevated temperature cohesiveness, it is characterised in that: combined by modified resin
Object and curing agent composition react to obtain；The modified resin composition includes: 70 parts of four-functional group epoxy resin, organosilicon ring
10 parts of oxygen resin, 10 parts of phenolic resin, 10 parts of polyurethane modified epoxy resin, 8 parts of dispersing agent；The curing agent composition packet
It includes: 89.4 parts of pyromellitic dianhydride, 10 parts of toughener, 0.6 part of compound accelerant.
2. the insulating materials according to claim 1 with high glass-transition temperature, elevated temperature cohesiveness, feature exist
In the dispersing agent is carboxymethyl cellulose/tartaric acid, preparation method are as follows: carboxymethyl cellulose is added to suitable go
In ionized water, stirring at normal temperature is to being completely dissolved；With 10% acetum adjust solution pH be 5-6, add ferrocene and
Tartaric acid, is warming up to 70-80 DEG C of stirring 2-3h, and grease occurs in reaction system；It is cooled to 30-40 DEG C, sodium chloride and sweet is added
Ammonia sodium taurocholate stirs 0.5-1h；It is cooled to room temperature, isolates grease, evaporation, crystallization obtain carboxymethyl cellulose/winestone
Acid.
3. the insulating materials according to claim 2 with high glass-transition temperature, elevated temperature cohesiveness, feature exist
In the mass ratio of: the carboxymethyl cellulose, ferrocene, tartaric acid, sodium chloride, NaGC be 30-40:1:20-30:2:
2。
4. a kind of preparation side with high glass-transition temperature, the insulating materials of elevated temperature cohesiveness as described in claim 1
Method, which comprises the following steps:
(1) preparation of modified resin composition: four-functional group epoxy resin is added in high speed dispersion storage tank, is preheated to 80 DEG C；
It is subsequently added into organosilicon epoxy resin, phenolic resin, polyurethane modified epoxy resin, 400-600r/min revolving speed is stirred
1h is cooled to 64-65 DEG C of addition dispersing agent, and 500r/min revolving speed is stirred 1h, then blowing；
(2) preparation of curing agent composition: pyromellitic dianhydride is added in reaction kettle, and stirring is warming up to 105 DEG C, is added
Toughener is cooled to 70-75 DEG C after 40-60r/min revolving speed insulated and stirred 3h, and compound accelerant, insulated and stirred 20- is added
30min；
(3) heating cure forms: by the composition of modified resin composition, curing agent and metallic silicon power according to mass ratio 100:
60:300 is mixed evenly, and the production of mutual inductor is carried out by way of vacuum pouring, using 80 DEG C of solidification 2h,
110 DEG C solidify 2h, 130 DEG C of curing process for solidifying 6-8h are solidified.
5. the preparation method according to claim 4 with high glass-transition temperature, the insulating materials of elevated temperature cohesiveness,
It is characterized in that, the metallic silicon power passes through modification, method of modifying are as follows: metallic silicon power is dispersed in dehydrated alcohol
In, 10-15min is impregnated, pH value of solution is adjusted with formic acid and PEG400 is then added to 5-6, and be heated to reflux state insulated and stirred
15-30min adds silane coupling agent, continues insulated and stirred 0.5-2h at reflux, cooled to room temperature, gained
Mixture is transferred to sealing and standing 2-6h in -5 DEG C of environment, and filtering, gained filter residue is sent into vacuum drier after being washed with dehydrated alcohol
Middle drying.
6. the preparation method according to claim 5 with high glass-transition temperature, the insulating materials of elevated temperature cohesiveness,
It is characterized by: the mass ratio of the metallic silicon power, PEG400, silane coupling agent is 10-15:1-5:1-5.
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| CN110185713A (en) * | 2019-07-10 | 2019-08-30 | 贝德科技有限公司 | A kind of Diesel engine pump check shaft coupling |
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