CN109825035A - A method of sensor sealed end insulating materials is prepared with nano zine oxide-is modified micaceous - Google Patents
A method of sensor sealed end insulating materials is prepared with nano zine oxide-is modified micaceous Download PDFInfo
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Abstract
The invention discloses a kind of with the modified micaceous method for preparing sensor sealed end insulating materials of nano zine oxide-, the nano zine oxide of KH550 moditied processing is mixed with acetone and is stirred evenly, end carboxyl super branched polyester, catalyst p-methyl benzenesulfonic acid, magnetic agitation is added, drying, grinding；Garrulous mica is rinsed with deionized water, is dried in vacuo, dopamine hydrochloride is added into buffer solution, dopamine solution is prepared, pretreated garrulous mica is added, stir process is rinsed well with deionized water, vacuum drying；Epoxy resin is heated, the short glass fiber of surface modification, the multi-walled carbon nanotube of acidizing pretreatment and end carboxyl super branched polyester graft nano zine oxide, modified micaceous are added, is uniformly mixed, is placed in ultrasonic disperse machinery in water-bath and stirs, curing agent, toughener, coupling agent KH550 is added, promotor is instilled after continuing stirring, vacuum defoamation is injected in mold, deaeration again, it takes out, is heating and curing, cooling the insulating materials.
Description
Technical field
The invention belongs to sensor fields, and in particular to a kind of to prepare sensor sealing with nano zine oxide-is modified micaceous
The method for holding insulating materials.
Background technique
Epoxy resin is used as high voltage electric equipment because having preferable electric insulating quality, lower-price characteristic extensively
Insulating materials.However, the insulation performance of corresponding high voltage electric equipment requires more and more with the continuous development of UHV transmission
Height, therefore the insulation performance for further increasing epoxy resin is particularly important.
Currently as the widely applied epoxy resin of insulating materials, although there are good electrical insulation properties,
It is not able to satisfy electric system requirement increasing for insulating reliability.The study found that dielectric aging is insulation breakdown
Major reason.Mixed nanometer modification is carried out to epoxy resin to have become to improve the resistance to electric branch ability of insulating materials
Research hotspot.
Summary of the invention
The purpose of the present invention is being directed to existing problem, a kind of modified micaceous preparation sensing of nano zine oxide-is provided
The method of device sealed end insulating materials, the insulating materials according to this method preparation have excellent insulation performance and heating conduction.
The present invention is achieved by the following technical solutions:
A method of sensor sealed end insulating materials is prepared with nano zine oxide-is modified micaceous, which is characterized in that including such as
Lower step:
(1) end carboxyl super branched polyester graft nano zine oxide:
The nano zine oxide of KH550 moditied processing and acetone 1:5-10 are mixed evenly, 0.025-0.035 parts of end carboxylics are added
Base hyper-branched polyester, 0.1-0.2 parts of catalyst p-methyl benzenesulfonic acid, the magnetic agitation 40-50min at 95-105 DEG C, in drying box
Middle drying, grinding；
(2) modified micaceous preparation:
6-9 parts of garrulous micas deionized water is rinsed 3-5 times, is dried in vacuo 10-12h at 40-45 DEG C, is added into buffer solution
Enter dopamine hydrochloride, compound concentration is the dopamine solution of 1-2%, and pretreated garrulous mica is added, and stir process 5-6h is used
Deionized water is rinsed well, is dried in vacuo 4-5h at 40-45 DEG C；
(3) preparation of insulating materials:
90-110 parts of epoxy resin are heated at 80-85 DEG C, add the short glass fiber of surface modification, acidizing pretreatment
Resulting material in multi-walled carbon nanotube and (1), (2), is uniformly mixed, and is placed in ultrasonic disperse machinery in 50-55 DEG C of water-bath and stirs
10-15min is mixed, 60-80 parts of curing agent, 15-20 parts of toughener, 0.75-1 parts of coupling agent KH550 are added, continues to stir 10-
1-2 parts of promotors are instilled after 15min, vacuum defoamation 20-25min injects in mold, then deaeration 10-15min, takes out, in 100-
Be heating and curing 4-6h in 140 DEG C of drying boxes, naturally cools to room temperature, the insulating materials is made.
Further, 5-7 parts of nano zine oxides KH550 moditied processing nano zine oxide in step (1): are put into 95-105
20-30min is mixed in drying and processing 6-8h in DEG C drying box, in mass ratio 1:2 and water, be added 250-350 part ethyl alcohol with
0.5-0.7 parts of Silane coupling agent KH550s, mechanical stirring ultrasonic wave stir 40-50min, in drying box heating, drying, grind
The nano zine oxide of KH550 moditied processing.
Further, the Tris-HCl buffer solution that buffer solution is pH 8-9 in step (2).
Further, it after 6-9 parts of short glass fibers being impregnated reaction with KH560 in step (3), is placed in acetone soln
After ultrasonic vibration rinses 1-2h, 4-5h is handled in 80-85 DEG C of air dry oven, obtains the short glass fiber of surface modification.
Further, multi-walled carbon nanotube acidizing pretreatment in step (3): it is 3 that multi-walled carbon nanotube, which is dissolved in volume ratio:
In 1 concentrated sulfuric acid/concentrated nitric acid nitration mixture, after ultrasonic vibration reacts 2-4h, with deionized water repeated flushing to neutrality, then it is clear with acetone
Filter 3-5 times is washed, dry 4-5h obtains the multi-walled carbon nanotube of acidizing pretreatment at 80-85 DEG C.
Further, epoxy resin is bisphenol A type epoxy resin E-51 in step (3), and curing agent is curing agent MTHPA,
Toughener is toughener LT-EP, and promotor is altax P-30.
The present invention has the advantage that compared with prior art
(1) coupling agent treatment nano zine oxide is cooperateed with using end carboxyl super branched polyester, epoxy resin is modified, surface connects
Branch has the nano zine oxide of end carboxyl super branched polyester degree of scatter in epoxy matrix good, between nano zine oxide and epoxy matrix
Even closer complexity is connected, and the higher trap of energy level occurs in interface area, further improves the insulation performance of composite material.
(2) auto polymerization has occurred in dopamine in mica interlayer crystal structure, and completely, dopamine is modified cloud to dopamine cladding
Mother imparts mica surface bumps shape characteristic, improves mica specific surface area, to be easier to form machinery with epoxy resin
Engagement has better composite strengthening effect.
(3) using short glass fiber, carbon nanotube as filler, composite doping modification, acidified place are carried out to epoxy resin
The carbon nanotube of reason is uniformly dispersed in the base, and agglomeration obviously weakens, while can be effectively improved glass fibre and matrix
Interfacial viscosity, composite material have good insulating properties and thermal conductivity；Nano zine oxide not only has to be received common to nanoparticle
There is field to cause nonlinear conductance characteristic and uvioresistant characteristic for rice characteristic, the dielectric material after can also making doping；
Using epoxy resin as matrix, with the short glass fiber of surface modification, the multi-walled carbon nanotube of acidizing pretreatment, carboxyl end group
Hyper-branched polyester engrafted nanometer zinc oxide, it is modified micaceous for doping particle, using blending method and auxiliary ultrasonic dispersion be prepared for
Composite insulating material, the modified particles of doping can improve the thermally conductive and dielectric properties of epoxy resin, increase internal trap quantity
And it is excellent in terms of promoting the resistance to electrical tree aging process of epoxy resin.
Specific embodiment
Embodiment 1
A method of sensor sealed end insulating materials is prepared with nano zine oxide-is modified micaceous, which is characterized in that including such as
Lower step:
(1) end carboxyl super branched polyester graft nano zine oxide:
The nano zine oxide of KH550 moditied processing and acetone 1:5 are mixed evenly, 0.025 part of addition is end carboxyl super branched
Polyester, 0.1 part of catalyst p-methyl benzenesulfonic acid, magnetic agitation 40min, is dried in drying box at 95-105 DEG C, grinding；
(2) modified micaceous preparation:
6 parts of garrulous micas deionized water is rinsed 3 times, 10h is dried in vacuo at 40-45 DEG C, DOPA is added into buffer solution
Amine hydrochlorate, the dopamine solution that compound concentration is 1%, is added pretreated garrulous mica, stir process 5h is rushed with deionized water
Wash clean is dried in vacuo 4h at 40-45 DEG C；
(3) preparation of insulating materials:
90 parts of epoxy resin are heated at 80-85 DEG C, add the short glass fiber of surface modification, the multi wall of acidizing pretreatment
Resulting material in carbon nanotube and (1), (2), is uniformly mixed, and is placed in ultrasonic disperse machinery in 50-55 DEG C of water-bath and stirs
60 parts of curing agent, 15 parts of toughener, 0.75 part of coupling agent KH550 is added in 10min, continues to instill 1 part of promotion after stirring 10min
Agent, vacuum defoamation 20min inject in mold, then deaeration 10min, take out, and be heating and curing 4h in 100-140 DEG C of drying box, from
It is so cooled to room temperature, the insulating materials is made.
Further, 5 parts of nano zine oxides KH550 moditied processing nano zine oxide in step (1): are put into 95-105 DEG C
20min is mixed in drying and processing 6h in drying box, in mass ratio 1:2 and water, and 250 parts of ethyl alcohol are added and 0.5 part silane coupled
Agent KH550, mechanical stirring ultrasonic wave stir 40min, in drying box heating, drying, grind KH550 moditied processing nanometer
Zinc oxide.
Further, the Tris-HCl buffer solution that buffer solution is pH 8 in step (2).
Further, it after 6 parts of short glass fibers being impregnated reaction with KH560 in step (3), is placed in acetone soln and surpasses
After flushing 1h is swung in acoustic shock, 4h is handled in 80-85 DEG C of air dry oven, obtains the short glass fiber of surface modification.
Further, multi-walled carbon nanotube acidizing pretreatment in step (3): it is 3 that multi-walled carbon nanotube, which is dissolved in volume ratio:
In 1 concentrated sulfuric acid/concentrated nitric acid nitration mixture, after ultrasonic vibration reacts 2h, cleaned with deionized water repeated flushing to neutrality, then with acetone
Filter 23, dry 4h obtains the multi-walled carbon nanotube of acidizing pretreatment at 80-85 DEG C.
Further, epoxy resin is bisphenol A type epoxy resin E-51 in step (3), and curing agent is curing agent MTHPA,
Toughener is toughener LT-EP, and promotor is altax P-30.
Embodiment 2
A method of sensor sealed end insulating materials is prepared with nano zine oxide-is modified micaceous, which is characterized in that including such as
Lower step:
(1) end carboxyl super branched polyester graft nano zine oxide:
The nano zine oxide of KH550 moditied processing and acetone 1:10 are mixed evenly, 0.035 part of addition is end carboxyl super branched
Polyester, 0.2 part of catalyst p-methyl benzenesulfonic acid, magnetic agitation 50min, is dried in drying box at 95-105 DEG C, grinding；
(2) modified micaceous preparation:
9 parts of garrulous micas deionized water is rinsed 5 times, 12h is dried in vacuo at 40-45 DEG C, DOPA is added into buffer solution
Amine hydrochlorate, the dopamine solution that compound concentration is 2%, is added pretreated garrulous mica, stir process 6h is rushed with deionized water
Wash clean is dried in vacuo 5h at 40-45 DEG C；
(3) preparation of insulating materials:
110 parts of epoxy resin are heated at 80-85 DEG C, add the short glass fiber of surface modification, acidizing pretreatment it is more
Resulting material in wall carbon nano tube and (1), (2), is uniformly mixed, and is placed in ultrasonic disperse machinery in 50-55 DEG C of water-bath and stirs
80 parts of curing agent, 20 parts of toughener, 1 part of coupling agent KH550 is added in 15min, continues to instill 2 parts of promotors after stirring 15min,
Vacuum defoamation 25min injects in mold, then deaeration 15min, takes out, and be heating and curing 6h in 100-140 DEG C of drying box, natural
It is cooled to room temperature, the insulating materials is made.
Further, 7 parts of nano zine oxides KH550 moditied processing nano zine oxide in step (1): are put into 95-105 DEG C
30min is mixed in drying and processing 8h in drying box, in mass ratio 1:2 and water, and 350 parts of ethyl alcohol are added and 0.7 part silane coupled
Agent KH550, mechanical stirring ultrasonic wave stir 50min, in drying box heating, drying, grind KH550 moditied processing nanometer
Zinc oxide.
Further, the Tris-HCl buffer solution that buffer solution is pH 9 in step (2).
Further, it after 9 parts of short glass fibers being impregnated reaction with KH560 in step (3), is placed in acetone soln and surpasses
After flushing 2h is swung in acoustic shock, 5h is handled in 80-85 DEG C of air dry oven, obtains the short glass fiber of surface modification.
Further, multi-walled carbon nanotube acidizing pretreatment in step (3): it is 3 that multi-walled carbon nanotube, which is dissolved in volume ratio:
In 1 concentrated sulfuric acid/concentrated nitric acid nitration mixture, after ultrasonic vibration reacts 4h, cleaned with deionized water repeated flushing to neutrality, then with acetone
Filtering 5 times, dry 5h obtains the multi-walled carbon nanotube of acidizing pretreatment at 80-85 DEG C.
Further, epoxy resin is bisphenol A type epoxy resin E-51 in step (3), and curing agent is curing agent MTHPA,
Toughener is toughener LT-EP, and promotor is altax P-30.
Comparative example 1
This comparative example 1 compared with Example 1, does not use end carboxyl super branched polyester graft modified Nano in step (1)
Zinc oxide, method and step in addition to this are all the same.
Comparative example 2
This comparative example 2 compared with Example 2, does not in step (3) carry out short glass fiber and multi-walled carbon nanotube
Pretreatment, method and step in addition to this are all the same.
Control group pure epoxy resin
In order to compare the performance of insulating materials produced by the present invention, to above-described embodiment 1, embodiment 2, comparative example 1, comparison
The corresponding insulating materials obtained of 2 method of embodiment and the corresponding pure epoxy resin of control group, carry out performance according to professional standard
Detection, specific correlation data are as shown in table 1 below:
Table 1
There is excellent insulation performance and heating conduction according to the insulating materials of the method for the present invention preparation, the medium of insulating materials damages
Consume factor be 0.58%, relative dielectric constant 4.8；It is not modified using end carboxyl super branched polyester graft in comparative example 1
Nano zine oxide causes the local starting voltage of insulating materials to reduce, but still rises better than the part of control group pure epoxy resin
Beginning voltage；Short glass fiber and multi-walled carbon nanotube are not pre-processed in comparative example 2, lead to insulating materials
Thermal coefficient reduces, but still is better than the heating conduction of control group pure epoxy resin.
Claims (6)
1. a kind of modified micaceous method for preparing sensor sealed end insulating materials of nano zine oxide-, which is characterized in that including
Following steps:
(1) end carboxyl super branched polyester graft nano zine oxide:
The nano zine oxide of KH550 moditied processing and acetone 1:5-10 are mixed evenly, 0.025-0.035 parts of end carboxylics are added
Base hyper-branched polyester, 0.1-0.2 parts of catalyst p-methyl benzenesulfonic acid, the magnetic agitation 40-50min at 95-105 DEG C, in drying box
Middle drying, grinding；
(2) modified micaceous preparation:
6-9 parts of garrulous micas deionized water is rinsed 3-5 times, is dried in vacuo 10-12h at 40-45 DEG C, is added into buffer solution
Enter dopamine hydrochloride, compound concentration is the dopamine solution of 1-2%, and pretreated garrulous mica is added, and stir process 5-6h is used
Deionized water is rinsed well, is dried in vacuo 4-5h at 40-45 DEG C；
(3) preparation of insulating materials:
90-110 parts of epoxy resin are heated at 80-85 DEG C, add the short glass fiber of surface modification, acidizing pretreatment
Resulting material in multi-walled carbon nanotube and (1), (2), is uniformly mixed, and is placed in ultrasonic disperse machinery in 50-55 DEG C of water-bath and stirs
10-15min is mixed, 60-80 parts of curing agent, 15-20 parts of toughener, 0.75-1 parts of coupling agent KH550 are added, continues to stir 10-
1-2 parts of promotors are instilled after 15min, vacuum defoamation 20-25min injects in mold, then deaeration 10-15min, takes out, in 100-
Be heating and curing 4-6h in 140 DEG C of drying boxes, naturally cools to room temperature, the insulating materials is made.
2. a kind of modified micaceous sensor sealed end insulating materials of preparing of nano zine oxide-according to claim 1
Method, which is characterized in that KH550 moditied processing nano zine oxide in step (1):
5-7 parts of nano zine oxides are put into drying and processing 6-8h in 95-105 DEG C of drying box, 1:2 in mass ratio and water are mixed
20-30min, is added 250-350 parts of ethyl alcohol and 0.5-0.7 parts of Silane coupling agent KH550s, and mechanical stirring ultrasonic wave stirs 40-
50min, in drying box heating, drying, grind KH550 moditied processing nano zine oxide.
3. a kind of modified micaceous sensor sealed end insulating materials of preparing of nano zine oxide-according to claim 1
Method, which is characterized in that buffer solution is the Tris-HCl buffer solution of pH 8-9 in step (2).
4. a kind of modified micaceous sensor sealed end insulating materials of preparing of nano zine oxide-according to claim 1
Method, which is characterized in that after 6-9 parts of short glass fibers are impregnated reaction with KH560 in step (3), be placed in acetone soln
After ultrasonic vibration rinses 1-2h, 4-5h is handled in 80-85 DEG C of air dry oven, obtains the short glass fiber of surface modification.
5. a kind of modified micaceous sensor sealed end insulating materials of preparing of nano zine oxide-according to claim 1
Method, which is characterized in that multi-walled carbon nanotube acidizing pretreatment in step (3):
Multi-walled carbon nanotube is dissolved in the concentrated sulfuric acid/concentrated nitric acid nitration mixture that volume ratio is 3:1, after ultrasonic vibration reacts 2-4h, is used
Deionized water repeated flushing is cleaned filter 23-5 times to neutrality, then with acetone, and dry 4-5h obtains acidizing pretreatment at 80-85 DEG C
Multi-walled carbon nanotube.
6. a kind of modified micaceous sensor sealed end insulating materials of preparing of nano zine oxide-according to claim 1
Method, which is characterized in that epoxy resin is bisphenol A type epoxy resin E-51 in step (3), and curing agent is curing agent MTHPA, is increased
Tough dose is toughener LT-EP, and promotor is altax P-30.
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