CN102391620A - Epoxy resin matrix nano-zinc oxide composite material and preparation method thereof - Google Patents
Epoxy resin matrix nano-zinc oxide composite material and preparation method thereof Download PDFInfo
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Abstract
The invention relates to an epoxy resin matrix nano-zinc oxide composite material and a preparation method of the epoxy resin matrix nano-zinc oxide composite material. The epoxy resin matrix nano-zinc oxide composite material comprises matrix resin, curing agent, accelerating agent and additive, wherein the matrix resin is epoxy resin, the curing agent is methy hexahydrophthalic anhydride, the accelerating agent is N, N- methylbenzylamine, and the additive is nano-zinc oxide; the epoxy resin matrix nano-zinc oxide composite material comprises the components in part by weight: 100 parts of the epoxy resin, 70-120 parts of the methy hexahydrophthalic anhydride, 1-4 parts of the N, N- methylbenzylamine, and 0.5-10 parts of the nano-zinc oxide; the preparation method of the epoxy resin matrix nano-zinc oxide composite material comprises the steps of: mixing the nano-zinc oxide, acetone, the epoxy resin, carrying out high-speed shearing and ultrasonic dispersion on the obtained mixture, removing the acetone by water bath, carrying out vacuum degassing after the curing agent and the accelerating agent are added, and curing by an oven. The epoxy resin matrix nano-zinc oxide composite material has the advantages of being excellent in dielectric property and especially strong in power frequency breaking down field strength. The preparation method of the epoxy resin matrix nano-zinc oxide composite material has the characteristic of low cost.
Description
Technical field
The invention belongs to the polymer based nanocomposites technical field, be specifically related to a kind of epoxy resin base nanometer zinc oxide matrix material and preparation method thereof.
Background technology
Epoxy resin is taken as a kind of insulating material with its good electric, mechanical property and is applied on all kinds of electric products; For example as the mould material of electrical apparatus insulations such as electric power mutual-inductor, X-former, insulator, the impregnating of the sealed insulation in the isolating switch, direct-current machine winding.Insulating material is the key condition that guarantees the normal operation of electrical equipment and electrical; The develop rapidly of power industry; Demands for higher performance to insulating material; So develop novel insulating material or original insulating material is carried out the improvement on the performance, all be the focus of countries in the world research all the time.
Pure epoxy resin often fragility is big, and the cracking resistance ability generally can add mineral filler improving its mechanical property, and reduce cost, but this can reduce its electric property.In the last few years; Along with the development of nanotechnology, nano material is widely used in various fields such as medical science, electronics, biology, chemical industry, under this overall situation; Also begin nano material is applied to insulating material in the electrical material field; In epoxy resins insulation, add nanometer inorganic filler, not only can improve and improve its mechanical property, and can expect to improve the dielectric properties of insulating material.
Summary of the invention
In order to overcome the shortcoming of above-mentioned prior art; The object of the present invention is to provide a kind of epoxy resin base nanometer zinc oxide matrix material and preparation method thereof; It is good that matrix material of the present invention has dielectric properties; The high advantage of power frequency breaking down field strength particularly, composite material and preparation method thereof of the present invention has characteristics with low cost.
In order to achieve the above object, the technical scheme that the present invention adopted is:
A kind of epoxy resin base nanometer zinc oxide matrix material; It is characterized in that: said matrix material is made up of matrix resin, solidifying agent, promotor and additive; Said matrix resin is an epoxy resin, and solidifying agent is a methyl hexahydrophthalic anhydride, and promotor is N; The N-dimethyl benzylamine; Additive is a nano zine oxide, and the weight part of each component is in this matrix material: epoxy resin is that 100 parts, methyl hexahydrophthalic anhydride are 70-120 part, N, and the N-dimethyl benzylamine is that 1-4 part and nano zine oxide are 0.5-10 part.
The weight part of each component is in the said matrix material: epoxy resin is that 100 parts, methyl hexahydrophthalic anhydride are 80-110 part, N, and the N-dimethyl benzylamine is that 1-3.5 part and nano zine oxide are 1-9.5 part.
Said epoxy resin is bisphenol A type epoxy resin.
A kind of method for preparing the said matrix material of claim 1 comprises the steps:
Step 1: nano zine oxide, acetone, epoxy resin mix high speed shear; At first 0.5-10 weight part surface is joined through the nano zinc oxide particles that coupling agent treatment is crossed in the middle of the mixing solutions of 40-60 parts by weight of epoxy resin thinner acetone and 100 parts by weight of epoxy resin; Stirring makes dispersion liquid not have the layering mixing, uses high speed shearing machine to handle dispersion liquid 15-60min with the rotating speed of 5000-20000r/min then;
Step 2: ultra-sonic dispersion, use ultrasonic generator to handle dispersion liquid 15-60min with power 500-1000W, frequency 20-25kHz the dispersion liquid after the processing of step 1 high speed shear;
Step 3: acetone is taken off in water-bath, the dispersion liquid that ultra-sonic dispersion was handled put into temperature be in 70 ℃ the water bath electronic stirring 2-4h to slough acetone;
Step 4: add the degassing of solidifying agent and promotor final vacuum; At first slough the solidifying agent methyl hexahydrophthalic anhydride that adds the 70-120 weight part in the dispersion liquid of acetone and the accelerant N of 1-4 weight part to step 3; The N-dimethyl benzylamine; And stir, being evacuated to relative vacuum degree-0.09--0.1Mpa then, postheating is to 30-50 ℃ and be incubated 30-60min to slough the bubble in the dispersion liquid;
Step 5: curing oven; At first the dispersion liquid after the deaeration is poured in the mould that releasing agent is handled; Heating is 80-105 ℃ and be incubated 2-4h in baking oven, continues to be heated to 120-140 ℃ and be incubated 6-10 hour, the promptly curable epoxy resin base nanometer zinc oxide matrix material that obtains then.
The said nano zinc oxide particles of step 1 was dried before joining mixing solutions, and bake out temperature is 100-130 ℃, and drying time is 5-10h.
The described coupling agent of step 1 is γ-An Bingjisanyiyangjiguiwan coupling agent (KH550), γ-(3; The 2-glycidoxy) one or more in methyltrimethoxy silane (KH560), γ-(methacryloxy) propyl trimethoxy silicane (KH570), the tetrabutyl titanate, if two or more then be any proportioning.
The described epoxy resin diluent acetone of step 1 is analytically pure acetone.
The described releasing agent of step 5 is that mass concentration is silicone grease/toluene solution of 5%.
The present invention has evenly spread to nano zinc oxide particles in the epoxy resin-base through high speed shear and ultrasonic method, and surface treatment mode has guaranteed dispersion and nanoparticle and epoxy resin molecular chain closely crosslinked of nano zinc oxide particles.Because the special effects that nanoparticle produces, for example interfacial effect etc. makes that only adding a small amount of nano zine oxide can make the nano composite material that dielectric properties are superior to pure epoxy resin.
Description of drawings
Fig. 1 is a composite material and preparation method thereof schema of the present invention.
Fig. 2 is a nanoparticle add-on when being 9.5 weight parts, the pattern sem photograph of epoxy resin base nanometer zinc oxide matrix material sample section of the present invention.
Fig. 3 is that the breaking down field strength of epoxy resin base nanometer zinc oxide matrix material of the present invention is with the nanoparticle content variation diagram.
Fig. 4 is the Weibull probability distribution graph of the power frequency breaking down field strength of epoxy resin base nanometer zinc oxide matrix material of the present invention.
Fig. 5 is the performance comparison diagram of the embodiment of the invention two prepared composite materials and pure epoxy resin and Comparative Examples prepared composite material.
Embodiment
Below in conjunction with accompanying drawing and specific embodiment the present invention is explained further details.
Embodiment one
As shown in Figure 1, the preparation method of this epoxy resin base nanometer zinc oxide matrix material may further comprise the steps:
Step 1: nano zine oxide, acetone, epoxy resin mix high speed shear; At first 0.5 weight part surface is dried 6h through the nano zinc oxide particles that KH560 handled under 100 ℃ temperature; Join then in the middle of the mixing solutions of 40 parts by weight of epoxy resin thinner acetone and 100 parts by weight of epoxy resin; Stirring makes dispersion liquid not have the layering mixing, uses high speed shearing machine to handle dispersion liquid 15min with the rotating speed of 5000r/min then;
Step 2: ultra-sonic dispersion, use ultrasonic generator to handle dispersion liquid 15min with power 500W, frequency 20kHz the dispersion liquid after the processing of step 1 high speed shear;
Step 3: acetone is taken off in water-bath, the dispersion liquid that ultra-sonic dispersion was handled put into temperature be in 70 ℃ the water bath electronic stirring 3h to slough acetone;
Step 4: add the degassing of solidifying agent and promotor final vacuum; At first slough the solidifying agent methyl hexahydrophthalic anhydride that adds 80 weight parts in the dispersion liquid of acetone and the accelerant N of 1 weight part to step 3; The N-dimethyl benzylamine; And stir, being evacuated to relative vacuum degree-0.09Mpa then, postheating to 40 ℃ also is incubated 30min to slough the bubble in the dispersion liquid;
Step 5: curing oven; At first pouring into the dispersion liquid after the deaeration through the releasing agent mass concentration is in the mould handled of 5% silicone grease/toluene solution; Heating is 80 ℃ and be incubated 2h in baking oven; Continue to be heated to 120 ℃ and be incubated 6 hours, the promptly curable epoxy resin base nanometer zinc oxide matrix material that obtains then.
Embodiment two
As shown in Figure 1, the preparation method of this epoxy resin base nanometer zinc oxide matrix material may further comprise the steps:
Step 1: nano zine oxide, acetone, epoxy resin mix high speed shear; At first 9.5 weight part surfaces are dried 8h through the nano zinc oxide particles that KH550 handled under 130 ℃ temperature; Join then in the middle of the mixing solutions of 60 parts by weight of epoxy resin thinner acetone and 100 parts by weight of epoxy resin; Stirring makes dispersion liquid not have the layering mixing, uses high speed shearing machine to handle dispersion liquid 40min with the rotating speed of 10000r/min then;
Step 2: ultra-sonic dispersion, use ultrasonic generator to handle dispersion liquid 30min with power 600W, frequency 24kHz the dispersion liquid after the processing of step 1 high speed shear;
Step 3: acetone is taken off in water-bath, the dispersion liquid that ultra-sonic dispersion was handled put into temperature be in 70 ℃ the water bath electronic stirring 4h to slough acetone;
Step 4: add the degassing of solidifying agent and promotor final vacuum; At first slough the solidifying agent methyl hexahydrophthalic anhydride that adds 90 weight parts in the dispersion liquid of acetone and the accelerant N of 2 weight parts to step 3; The N-dimethyl benzylamine; And stir, being evacuated to relative vacuum degree-0.095Mpa then, postheating to 40 ℃ also is incubated 45min to slough the bubble in the dispersion liquid;
Step 5: curing oven; At first pouring into the dispersion liquid after the deaeration through the releasing agent mass concentration is in the mould handled of 5% silicone grease/toluene solution; Heating is 80 ℃ and be incubated 4h in baking oven; Continue to be heated to 120 ℃ and be incubated 6 hours, the promptly curable epoxy resin base nanometer zinc oxide matrix material that obtains then.
Embodiment three
As shown in Figure 1, the preparation method of this epoxy resin base nanometer zinc oxide matrix material may further comprise the steps:
Step 1: nano zine oxide, acetone, epoxy resin mix high speed shear; The nano zinc oxide particles of at first 6 weight part surfaces being crossed than combination treatment arbitrarily through KH570 and tetrabutyl titanate is dried 10h under 130 ℃ temperature; Join then in the middle of the mixing solutions of 60 parts by weight of epoxy resin thinner acetone and 100 parts by weight of epoxy resin; Stirring makes dispersion liquid not have the layering mixing, uses high speed shearing machine to handle dispersion liquid 45min with the rotating speed of 15000r/min then;
Step 2: ultra-sonic dispersion, use ultrasonic generator to handle dispersion liquid 45min with power 800W, frequency 22kHz the dispersion liquid after the processing of step 1 high speed shear;
Step 3: acetone is taken off in water-bath, the dispersion liquid that ultra-sonic dispersion was handled put into temperature be in 70 ℃ the water bath electronic stirring 4h to slough acetone;
Step 4: add the degassing of solidifying agent and promotor final vacuum; At first slough the solidifying agent methyl hexahydrophthalic anhydride that adds 100 weight parts in the dispersion liquid of acetone and the accelerant N of 3 weight parts to step 3; The N-dimethyl benzylamine; And stir, being evacuated to relative vacuum degree-0.09Mpa then, postheating to 50 ℃ also is incubated 60min to slough the bubble in the dispersion liquid;
Step 5: curing oven; At first pouring into the dispersion liquid after the deaeration through the releasing agent mass concentration is in the mould handled of 5% silicone grease/toluene solution; Heating is 100 ℃ and be incubated 4h in baking oven; Continue to be heated to 130 ℃ and be incubated 10 hours, the promptly curable epoxy resin base nanometer zinc oxide matrix material that obtains then.
Comparative Examples
The preparation method of this epoxy resin base nanometer zinc oxide matrix material has omitted high speed shear shown in Figure 1 and ultra-sonic dispersion process, has adopted following steps:
Step 1: nano zine oxide, acetone, epoxy resin mix; At first 9.5 weight part surfaces are dried 8h through the nano zinc oxide particles that KH550 handled under 130 ℃ temperature; Join then in the middle of the mixing solutions of acetone and 100 parts by weight of epoxy resin of 60 weight parts; Stirring makes dispersion liquid not have the layering mixing
Step 2: acetone is taken off in water-bath, the dispersion liquid that ultra-sonic dispersion was handled put into temperature be in 70 ℃ the water bath electronic stirring 4h to slough acetone.
Step 3: add the degassing of solidifying agent and promotor final vacuum; At first slough the solidifying agent methyl hexahydrophthalic anhydride that adds 90 weight parts in the dispersion liquid of acetone and the accelerant N of 2 weight parts to step 2; The N-dimethyl benzylamine; And stir, being evacuated to relative vacuum degree-0.095MPa then, postheating to 40 ℃ also is incubated 45min to slough the bubble in the dispersion liquid;
Step 4: curing oven; At first pouring into the dispersion liquid after the deaeration through the releasing agent mass concentration is in the mould handled of 5% silicone grease/toluene solution; Be heated to 80 ℃ and be incubated 4h then; Continue to be heated to 120 ℃ and be incubated 6 hours at last, solidify and obtain epoxy resin base nanometer zinc oxide matrix material.
As shown in Figure 2, the profile scanning Electronic Speculum figure of the epoxy resin base nanometer zinc oxide matrix material that instance two is prepared can find out that from figure particle is nano level basically and distributes.
As shown in Figure 3, mass percent shown in the figure is the mass ratio of nano zinc oxide particles quality and epoxy resin solidifying system, for example when the nanoparticle add-on is 9.5 weight parts; Pairing epoxy resin is 100 weight parts, and solidifying agent is 90 weight parts, so the massfraction of nanoparticle is 9.5/ (100+90)=5%; Can see from figure; The nanoparticle of low levels is also little to the influence of the power frequency uniform field breaking down field strength of epoxy resin, but when content was high, the power frequency breaking down field strength began to improve; When the content of nanoparticle was 5%, the breaking down field strength of matrix material was the highest.
As shown in Figure 4, as can be seen from the figure, no matter puncture and the high probability puncture at low probability, 5% content nano zinc oxide particles improves all comparatively obvious to the breaking down field strength of epoxy resin.
As shown in Figure 5; The dielectric loss that from figure, can find out Comparative Examples prepared composite material rises; Resistivity, voltage breakdown then descend; The dielectric properties variation, and the prepared epoxy resin base nanometer zinc oxide matrix material of Comparative Examples is identical with the material mixture ratio shown in the instance two, but omitted high speed shear and ultransonic dispersion process.
Epoxy resin base nanometer zinc oxide matrix material dielectric properties of the present invention are good; When the nano zinc oxide particles consumption is 9.5 weight parts, it is best that its dielectric properties reach, and power frequency uniform field breaking down field strength improves 37.3%; 5% probability breaking down field strength improves 43.4%; Branch doubles breakdown time, and loss factor only has slight rising under the power frequency simultaneously, and MV is from 3.6 * 10
-3Rise to 4.2 * 10
-3, volume specific resistance remains unchanged basically, 5 * 10
14～2 * 10
15Change in the Ω m scope.
Epoxy resin base nanometer zinc oxide matrix material of the present invention reaches the product of on its basis, doing suitable additives; Can be used as the insulating material of multiclass electric product; Like the mould material as electrical apparatus insulations such as electric power mutual-inductor, X-former, insulators, the impregnating of the sealed insulation in the isolating switch, direct-current machine winding.
Claims (9)
1. epoxy resin base nanometer zinc oxide matrix material; It is characterized in that: said matrix material is made up of matrix resin, solidifying agent, promotor and additive; Said matrix resin is an epoxy resin, and solidifying agent is a methyl hexahydrophthalic anhydride, and promotor is N; The N-dimethyl benzylamine; Additive is a nano zine oxide, and the weight part of each component is in this matrix material: epoxy resin is that 100 parts, methyl hexahydrophthalic anhydride are 70-120 part, N, and the N-dimethyl benzylamine is that 1-4 part and nano zine oxide are 0.5-10 part.
2. matrix material according to claim 1; It is characterized in that: the weight part of each component is in the said matrix material: epoxy resin is that 100 parts, methyl hexahydrophthalic anhydride are 80-110 part, N, and the N-dimethyl benzylamine is that 1-3.5 part and nano zine oxide are 0.5-10 part.
3. matrix material according to claim 1 and 2 is characterized in that: said epoxy resin is bisphenol A type epoxy resin.
4. a method for preparing the said matrix material of claim 1 comprises the steps:
Step 1: nano zine oxide, acetone, epoxy resin mix high speed shear; At first 0.5-10 weight part surface is joined through the nano zinc oxide particles that coupling agent treatment is crossed in the middle of the mixing solutions of 40-60 parts by weight of epoxy resin thinner acetone and 100 parts by weight of epoxy resin; Stirring makes dispersion liquid not have the layering mixing, uses high speed shearing machine to handle dispersion liquid 15-60min with the rotating speed of 5000-20000r/min then;
Step 2: ultra-sonic dispersion, use ultrasonic generator to handle dispersion liquid 15-60min with power 500-1000W, frequency 20-25kHz the dispersion liquid after the processing of step 1 high speed shear;
Step 3: acetone is taken off in water-bath, the dispersion liquid that ultra-sonic dispersion was handled put into temperature be in 70 ℃ the water bath electronic stirring 2-4h to slough acetone;
Step 4: add the degassing of solidifying agent and promotor final vacuum; At first slough the solidifying agent methyl hexahydrophthalic anhydride that adds the 70-120 weight part in the dispersion liquid of acetone and the accelerant N of 1-4 weight part to step 3; The N-dimethyl benzylamine; And stir, being evacuated to relative vacuum degree-0.09--0.1Mpa then, postheating is to 30-50 ℃ and be incubated 30-60min to slough the bubble in the dispersion liquid;
Step 5: curing oven; At first the dispersion liquid after the deaeration is poured in the mould that releasing agent is handled; Heating is 80-105 ℃ and be incubated 2-4h in baking oven, continues to be heated to 120-140 ℃ and be incubated 6-10 hour, the promptly curable epoxy resin base nanometer zinc oxide matrix material that obtains then.
5. preparation method according to claim 4 is characterized in that: the said nano zinc oxide particles of step 1 was dried before joining mixing solutions, and bake out temperature is 100-130 ℃, and drying time is 5-10h.
6. preparation method according to claim 4; It is characterized in that: the described coupling agent of step 1 is γ-An Bingjisanyiyangjiguiwan coupling agent (KH550), γ-(3; The 2-glycidoxy) one or more in methyltrimethoxy silane (KH560), γ-(methacryloxy) propyl trimethoxy silicane (KH570), the tetrabutyl titanate, if two or more then be any proportioning.
7. preparation method according to claim 4 is characterized in that: the described epoxy resin diluent acetone of step 1 is analytically pure acetone.
8. preparation method according to claim 4 is characterized in that: the described releasing agent of step 5 is that mass concentration is silicone grease/toluene solution of 5%.
9. preparation method according to claim 4 is characterized in that: comprise the steps:
Step 1: nano zine oxide, acetone, epoxy resin mix high speed shear; At first 9.5 weight part surfaces are dried 8h through the nano zinc oxide particles that KH550 handled under 130 ℃ temperature; Join then in the middle of the mixing solutions of 60 parts by weight of epoxy resin thinner acetone and 100 parts by weight of epoxy resin; Stirring makes dispersion liquid not have the layering mixing, uses high speed shearing machine to handle dispersion liquid 40min with the rotating speed of 10000r/min then;
Step 2: ultra-sonic dispersion, use ultrasonic generator to handle dispersion liquid 30min with power 600W, frequency 24kHz the dispersion liquid after the processing of step 1 high speed shear;
Step 3: acetone is taken off in water-bath, the dispersion liquid that ultra-sonic dispersion was handled put into temperature be in 70 ℃ the water bath electronic stirring 4h to slough acetone;
Step 4: add the degassing of solidifying agent and promotor final vacuum; At first slough the solidifying agent methyl hexahydrophthalic anhydride that adds 90 weight parts in the dispersion liquid of acetone and the accelerant N of 2 weight parts to step 3; The N-dimethyl benzylamine; And stir, being evacuated to relative vacuum degree-0.095Mpa then, postheating to 40 ℃ also is incubated 45min to slough the bubble in the dispersion liquid;
Step 5: curing oven; At first pouring into the dispersion liquid after the deaeration through the releasing agent mass concentration is in the mould handled of 5% silicone grease/toluene solution; Heating is 80 ℃ and be incubated 4h in baking oven; Continue to be heated to 120 ℃ and be incubated 6 hours, the promptly curable epoxy resin base nanometer zinc oxide matrix material that obtains then.
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