CN107964380A - A kind of Non-Gaussian Distribution aluminium hydrate powder and its preparation method and application - Google Patents
A kind of Non-Gaussian Distribution aluminium hydrate powder and its preparation method and application Download PDFInfo
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- CN107964380A CN107964380A CN201711462861.1A CN201711462861A CN107964380A CN 107964380 A CN107964380 A CN 107964380A CN 201711462861 A CN201711462861 A CN 201711462861A CN 107964380 A CN107964380 A CN 107964380A
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- 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
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- 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
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- 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
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
- C08K2003/2227—Oxides; Hydroxides of metals of aluminium
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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/002—Physical properties
- C08K2201/003—Additives being defined by their diameter
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- 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
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Abstract
The invention discloses a kind of Non-Gaussian Distribution aluminium hydrate powder, is mixed by the aluminium hydrate powder that particle diameter is 2 μm and the aluminium hydrate powder that particle diameter is 18 μm.The mixing quality ratio of 2 μm of aluminium hydrate powders and 18 μm of aluminium hydrate powders is 11：8~11：4, it is preferably 11：7~11：5, it is most preferably 2:1.A kind of application of Non-Gaussian Distribution aluminium hydrate powder, adds in the preparation of bicomponent epoxy resin electron pouring sealant component A in using Non-Gaussian Distribution aluminium hydrate powder as filler.Product of the present invention can be effectively improved the problem of low-viscosity and anti-settling mutual exclusion in epoxy-resin systems, it is effectively improved it and merges performance, when being used for epoxy resin embedding adhesive as filler, it can obtain low-viscosity and non-setting product, the usage time and mobile performance for making product all significantly improve, and practicality is stronger.
Description
Technical field
The present invention relates to a kind of Non-Gaussian Distribution aluminium hydrate powder and its preparation method and application, belong to electron pouring sealant skill
Art field.
Background technology
With the rapid development of electronic technology, its speed of service is getting faster, electronic component and logic circuit etc. all tend to
In miniaturization and densification development, the raising of power is run in addition so that the heat that electronic product unit area produces constantly increases
Add, at this moment the heat dispersal situations of electronic device with regard to it is particularly important that；If heat cannot distribute in time, it will localized hyperthermia is formed, into
And influence the stability and service life of electric appliance., can not only after being packaged using electron pouring sealant to electronic component
Enough heat dissipations well, moreover it is possible to play moisture-proof, dust-proof and shockproof effect, therefore the application in electronic product is more and more extensive.
At present, electronic component adds aluminium hydrate powder as filler by the use of usual demand in epoxy resin embedding adhesive, to change
The viscosity and anti-sedimentation effect of kind casting glue.The particle diameter of aluminium hydrate powder and the viscosity of casting glue are in normal distribution：Aluminium hydroxide
The particle diameter of powder is smaller, and specific surface area is bigger, and the contact area of powder and epoxy resin is bigger, binding site is more, casting glue it is glutinous
Degree is higher, is not likely to produce precipitation；Conversely, the particle diameter of aluminium hydrate powder is bigger, the viscosity of casting glue is lower but easily sinks
Form sediment.In general, in order to obtain more preferable embedding effect, it usually needs casting glue system it is homogeneous, avoid precipitation on the basis of
With lower viscosity, strengthen its mobile performance.Therefore, embedding gumminess but also sludge proof hydrogen-oxygen can be improved by preparing one kind
Change aluminium powder, be of great significance to improving the filler systems of epoxy resin embedding adhesive, reducing casting glue manufacturing cost.
The content of the invention
The technical problem to be solved in the present invention is to provide a kind of Non-Gaussian Distribution aluminium hydrate powder and preparation method thereof and answer
With to solve the problems, such as low-viscosity and anti-precipitability mutual exclusion in epoxy resin embedding adhesive system；By Non-Gaussian Distribution aluminium hydroxide
Powder is added in epoxy resin embedding adhesive system as filler, can obtain low-viscosity and non-setting epoxy resin embedding adhesive.
In order to solve the above technical problems, the technical solution used in the present invention is：
A kind of Non-Gaussian Distribution aluminium hydrate powder, by the aluminium hydrate powder that particle diameter is 2 μm and the aluminium hydrate powder that particle diameter is 18 μm
Mix.The mixing quality ratio of 2 μm of aluminium hydrate powders and 18 μm of aluminium hydrate powders is 11：8~11：4, it is preferably 11：7
~11：5, it is most preferably 2:1.
A kind of preparation method of Non-Gaussian Distribution aluminium hydrate powder, comprises the steps of：
A, crush：Aluminium hydroxide is crushed using original powder pulverizer, obtains the aluminium hydroxide of 2 μm and 18 μm two kinds of specifications
Powder；
B, screen：The aluminium hydrate powders of 2 μm and 18 μm is screened respectively with powder classification vibrating screen under room temperature, to ensure powder
Body uniform particle diameter；
C, mix：2 μm and 18 μm of aluminium hydrate powder is added in 360 ° of rotary blenders in mass ratio and is mixed, mixing temperature is
90 ± 2 DEG C, incorporation time is 2 ± 0.5h；It is to be mixed uniform up to Non-Gaussian Distribution aluminium hydrate powder.
A kind of application of Non-Gaussian Distribution aluminium hydrate powder, is using Non-Gaussian Distribution aluminium hydrate powder as filler
Preparation for bicomponent epoxy resin electron pouring sealant.
The component A and B component that the bicomponent epoxy resin electron pouring sealant is preserved including separation, component A and B component
Mass ratio is 100：20~25；The Non-Gaussian Distribution aluminium hydrate powder is added into component A as filler.
The component A includes following component by weight percentage：Epoxy resin 35% ~ 50%, diluent 5% ~ 15% are non-
Normal distribution aluminium hydrate powder 42% ~ 60%, color 1% ~ 5%, defoamer 0 ~ 1%；Preferably comprise by weight percentage such as the following group
Part：Epoxy resin 40% ~ 45%, diluent 5% ~ 8%, Non-Gaussian Distribution aluminium hydrate powder 45% ~ 50%, color 1% ~ 5%, defoamer 0 ~
1%。
Wherein, the epoxy resin be selected from bisphenol A type epoxy resin, bisphenol f type epoxy resin, cycloaliphatic epoxy resin,
Any one in aliphatic epoxy resin；The diluent is selected from butyl glycidyl ether, carbon lauryl diglycidyl ether
Or any one in benzyl glycidyl ether；The defoamer is defoamer HP-512.
The B component is polyamide curing agent.
It is using beneficial effect caused by above-mentioned technical proposal：
The present invention provides a kind of Non-Gaussian Distribution aluminium hydrate powder and its preparation method and application, which can have
Effect improves in epoxy-resin systems low-viscosity and the problem of anti-settling mutual exclusion, is effectively improved its and merges performance, as filler
During for epoxy resin embedding adhesive, low-viscosity and non-setting product can be obtained, makes the usage time and mobile performance of product
All significantly improve, practicality is stronger；And can largely be added in epoxy resin embedding adhesive, reduce epoxy resin embedding adhesive
Production cost, be conducive to industrial amplification production.
The preparation method of the Non-Gaussian Distribution aluminium hydrate powder is simple, using equipment is conventional, preparation condition is not harsh and
Easy to control, industrialization large-scale production, clean environment firendly are very suitable for.
The filler of component A uses in Non-Gaussian Distribution aluminium hydrate powder is as bicomponent epoxy resin electron pouring sealant
When, gained component A has the characteristics that low-viscosity and is not easy to precipitate at the same time, and homogeneity and mobility are strengthened at the same time, so that
Extend two kinds of components is used in mixed way the time；Meanwhile the addition of Non-Gaussian Distribution aluminium hydrate powder is to the breakdown potential of component A
The performances such as pressure, fire-retardant rank, dielectric constant, glass transition temperature do not have an impact, and ensure that epoxy resin electronic pouring sealant
With excellent performance parameter and good usage experience.
Brief description of the drawings
Fig. 1 is the grain size distribution of 1 gained Non-Gaussian Distribution aluminium hydrate powder of the embodiment of the present invention；
Fig. 2 is the aluminium hydrate powder grain size distribution that commercially available median is 8 μm.
Embodiment
Below in conjunction with specific embodiment, the present invention is further described.
A kind of Non-Gaussian Distribution aluminium hydrate powder, by the aluminium hydrate powder that particle diameter is 2 μm and the hydroxide that particle diameter is 18 μm
Aluminium powder mixes；Both mixing quality ratios are 11：8~11：4, it is preferably 11：7~11：5, it is most preferably 2:1.
The preparation method of the Non-Gaussian Distribution aluminium hydrate powder, comprises the steps of：
A, crush：Aluminium hydroxide is crushed using original powder pulverizer, obtains the aluminium hydroxide of 2 μm and 18 μm two kinds of specifications
Powder；
B, screen：The aluminium hydrate powder of 2 μm and 18 μm is sieved respectively with 960 times/min with powder classification vibrating screen under room temperature
Choosing, to ensure that diameter of particle is homogeneous；
C, mix：2 μm and 18 μm of aluminium hydrate powder is added in 360 ° of rotary blenders in mass ratio and is mixed, mixing temperature 90
± 2 DEG C, 2 ± 0.5h is mixed, after mixing up to Non-Gaussian Distribution aluminium hydrate powder.
The application of the Non-Gaussian Distribution aluminium hydrate powder, is to be used for using Non-Gaussian Distribution aluminium hydrate powder as filler
The preparation of bicomponent epoxy resin electron pouring sealant.
The bicomponent epoxy resin electron pouring sealant includes the component A and B component that separation preserves, wherein, component A is filling
Sealing, Non-Gaussian Distribution aluminium hydrate powder are added into component A as filler；The B component is polyamide curing agent, goes forward side by side one
Step is preferably T31 curing agent, 650 curing agent or 593 curing agent.
The mass ratio of the component A casting glue and B component curing agent is 100：20 ~ 25, it is preferably 100：23.
The component A includes following component by weight percentage：Epoxy resin 35% ~ 50%, diluent 5% ~ 15%, hydrogen
Alumina powder 42% ~ 60%, color 1% ~ 5%, defoamer 0 ~ 1%；
Preferably：Epoxy resin 40% ~ 45%, diluent 5% ~ 8%, aluminium hydrate powder 45% ~ 50%, color 1% ~ 5%, defoamer 0 ~
1%；
Most preferably：Epoxy resin 42% ~ 44%, diluent 6% ~ 7%, aluminium hydrate powder 46% ~ 48%, color 2% ~ 4%, defoamer
0.2~0.6%。
In component A：
The epoxy resin is bisphenol A type epoxy resin, bisphenol f type epoxy resin, cycloaliphatic epoxy resin, aliphatic epoxy tree
One or more in fat, and the epoxide number of epoxy resin is 0.48 ~ 0.60 eq/100g, 40 DEG C of viscosity≤2500mPa
S, volatile matter≤2%.
The diluent is in butyl glycidyl ether, carbon lauryl diglycidyl ether or benzyl glycidyl ether
Any one.
When diluent is butyl glycidyl ether, its colourity APHA≤20, viscosity（25℃）≤ 2mPa.s, easy saponification chlorine
Eq/100g≤0.01, inorganic chlorine eq/100g≤0.001；
When diluent is carbon lauryl diglycidyl ether, its colourity APHA≤30, viscosity（25℃）2mPa.s ~ 8mpa.s,
Easy saponification chlorine eq/100g≤0.01, inorganic chlorine eq/100g≤0.005；
When diluent is benzyl glycidyl ether, its colourity APHA≤50, viscosity（25℃）2mPa.s ~ 8mpa.s, easy saponification
Chlorine eq/100g≤0.01, inorganic chlorine eq/100g≤0.005.
The defoamer selects defoamer HP-512, its appearance is canescence translucent liquid, and 25 DEG C of viscosity are 800 cps
~ 1500cps, 25 DEG C of proportions are 0.99 ~ 1.
The preparation method of above-mentioned bicomponent epoxy resin casting glue comprises the following steps：
A, component A is prepared：
（1）Precise epoxy resin, diluent, Non-Gaussian Distribution aluminium hydrate powder, color and defoamer in proportion, are then pressed
Order adds epoxy resin, diluent, color and defoamer in reactor；
（2）Liquid components in reactor are stirred into 1 ± 0.5h of reaction at normal temperatures；
（3）By Non-Gaussian Distribution aluminium hydrate powder when preliminary drying 1 is small under the conditions of 90 ± 2 DEG C；
（4）Pre-baked Non-Gaussian Distribution aluminium hydrate powder is added in the liquid components that stir evenly, continue stirring 1.5 ±
0.5h；
（5）Reaction solution in reactor is transferred in vacuum defoaming device, deaeration 0.5h is left under the conditions of -0.1 ± 0.01MPa
The right side, that is, complete the preparation of component A；
B, when not in use, component A and B component separation storage, storage temperature are not higher than 40 DEG C；
C, when needing to use epoxy resin embedding adhesive, component A and B component is proportionally added into container at 25 DEG C and stirred
It is uniformly mixed, then vacuum defoamation, up to epoxy resin embedding adhesive；Gained casting glue can be at 25 DEG C in being used in 120min.
1 ~ embodiment of the following examples 5 is the preparation embodiment of Non-Gaussian Distribution aluminium hydrate powder.
Embodiment 1
The Non-Gaussian Distribution aluminium hydrate powder is mixed by the aluminium hydrate powder that particle diameter is 2 μm and the aluminium hydrate powder that particle diameter is 18 μm
Conjunction forms, both mixing quality ratios are 2:1.
Specifically preparation method is：
A, crush：Aluminium hydroxide is crushed using original powder pulverizer, obtains the aluminium hydroxide of 2 μm and 18 μm two kinds of specifications
Powder；
B, screen：The aluminium hydrate powder of 2 μm and 18 μm is sieved respectively with 960 times/min with powder classification vibrating screen under room temperature
Choosing, to ensure that diameter of particle is homogeneous；
C, mix：By 2 μm and 18 μm of aluminium hydrate powder in mass ratio 2:Mixed in 1 360 ° of rotary blenders of addition, mixing temperature
90 ± 2 DEG C of degree, mixes after 2h up to Non-Gaussian Distribution aluminium hydrate powder.
The Non-Gaussian Distribution aluminium hydrate powder prepared using LS-POP (9) laser particle size analyzers to embodiment 1 carries out grain
Footpath distribution tests, test chart are shown in Fig. 1, include two high-selenium corn peaks.By the peak area in Fig. 1 it can be calculated that the hydroxide
The average grain diameter of aluminium powder is about 7.3 μm.
2 ~ embodiment of embodiment 5
The formula of the Non-Gaussian Distribution aluminium hydrate powder of 2 ~ embodiment of embodiment 5 is shown in Table 1, and its preparation method is the same as in embodiment 1
Preparation method is identical.
1 Non-Gaussian Distribution aluminium hydrate powder formula of table and average grain diameter
Note：Grain size distribution test equipment and test method, average grain diameter computational methods are same as Example 1, grain size distribution
2 ~ embodiment of display embodiment, 5 product includes two high-selenium corn peaks.
Mixed below using the Non-Gaussian Distribution aluminium hydrate powder prepared by 1 ~ embodiment of embodiment 5 as filler and base resin
Close, prepare the component A of simple version, and carry out viscosity and settling property test.
1st, test method
Resin based on the commercially available E51 epoxy resin of five parts of 50g is taken at 25 DEG C, is added respectively into five parts of base resins
Non-Gaussian Distribution aluminium hydrate powder prepared by 1 ~ embodiment of 75g embodiments 5, labeled as S1 ~ S5, it is tested after being uniformly mixed
Viscosity and settling property.
2nd, method for testing performance
Viscosity test method：With reference to GB2794-2013；
Settling property test method：Take 200 grams of epoxy resin component A samples to enclose sample bottle, 100h is stood at 80 DEG C, observe
Whether precipitation is had.
3rd, test result
4th, conclusion
By data above as can be seen that the Non-Gaussian Distribution aluminium hydrate powder prepared by 1 ~ embodiment of embodiment 5 adds basis
After resin, relatively low viscosity and good sedimentation function can be obtained at the same time, and the viscosity under the conditions of its 40 DEG C is not higher than 34000
MPa.s, and produced in the case where 80 DEG C, 100h are stood without precipitation.
The Non-Gaussian Distribution aluminium hydrate powder prepared by Example 1 is made respectively with common commercially available aluminium hydrate powder below
Mixed for filler with base resin, prepare the component A of simple version, and tested its viscosity and settling property, contrasted.
1st, sample collocation method
Resin based on the commercially available E51 epoxy resin of five parts of 50g is taken at 25 DEG C, is added respectively into five parts of base resins
The hydrogen of the Non-Gaussian Distribution aluminium hydrate powder of the preparation of 75g embodiments 1,8 μm of aluminium hydrate powder, the median of 6 μm of median
Alumina powder, the aluminium hydrate powder of 15 μm of median, the aluminium hydrate powder of 25 μm of median, be respectively labeled as S1, D1,
D2、D3、D4；Its viscosity and settling property are tested after being uniformly mixed.
2nd, method for testing performance
Viscosity test method：With reference to GB2794-2013；
Settling property test method：Take 200 grams of epoxy resin component A samples to enclose sample bottle, 100h is stood at 80 DEG C, observe
Whether precipitation is had.
3rd, test result
4th, conclusion
Although the aluminium hydrate powder median added in S1, D1, D2 is not much different, the component A viscosity of D1, D2 are notable
The viscosity of viscosity higher than S1, especially D1 almost reaches twice of S1 soon；And hydrogen of the aluminium hydrate powder particle diameter of D2 only than S1
Alumina powder particle diameter is 0.7 μm big, but has had microprecipitation appearance in settling property test, can not meet wanting for homogeneity
Ask.
D3 and D4 uses the larger aluminium hydrate powder of particle diameter, and as filler, compared with D1, D2, its viscosity improves notable, D3
Viscosity is more than S1 viscositys, D4 viscositys are less than S1 viscositys；But the two comparative examples can not all meet settling property test request,
There is significantly precipitation.
As it can be seen that tetra- comparative examples of D1 ~ D4 use common aluminium hydrate powder, with the reduction of its particle diameter, to compare table as filler
Area increases, and the contact area of aluminium hydrate powder and epoxy resin is bigger, and viscosity is bigger；And once viscosity increases, its precipitability
It will can be affected.And the Non-Gaussian Distribution aluminium hydrate powder prepared by embodiment 1 can be effectively reduced the viscosity of component A
Can effectively avoid the occurrence of precipitation again, its homogeneity, mobility and processing performance at the same time be improved significantly.
6 ~ embodiment of the following examples 10 is the Application Example of Non-Gaussian Distribution aluminium hydrate powder.
In the examples below that, used raw material producer and its specification see the table below.
| Material name | Producer | Specification |
| E51 epoxy resin | Guangdong HongChang Electronic Materials Co., Ltd | Technical grade, 20kg/bucket |
| Bisphenol A type epoxy resin E54 | Wuxi resin processing plant | Technical grade, 20kg/bucket |
| Cycloaliphatic epoxy resin | Wuhan Senmao Fine Chemical Co., Ltd. | Technical grade, 20KG/bucket |
| Bisphenol f type epoxy resin | South Asia epoxy resin Co., Ltd | Technical grade, 220KG/ barrels |
| Butyl glycidyl ether | New far Chemical Industry Co., Ltd. of Anhui | Technical grade, 20kg modeling buckets or 200kg metal buckets packaging |
| Carbon lauryl diglycidyl ether | New far Chemical Industry Co., Ltd. of Anhui | Technical grade, 20kg modeling buckets or 200kg metal buckets packaging |
| Benzyl glycidyl ether | New far Chemical Industry Co., Ltd. of Anhui | Technical grade, 20kg modeling buckets or 200kg metal buckets packaging |
| Blue color | From processing | Technical grade, 25kg/ barrels |
| HP-512 defoamers | The chemical Science and Technology Ltd. of Guangzhou Hope | Technical grade, 25kg/ barrels |
Embodiment 6
A kind of bicomponent epoxy resin electron pouring sealant containing Non-Gaussian Distribution aluminium hydrate powder, is 100 by mass ratio:23
Component A and B component are formed, and the B component is T31 curing agent, and the component A includes following component：
Commercially available E51 epoxy resin 420g, diluent butyl glycidyl ether 50g, the Non-Gaussian Distribution aluminium hydrate powder of embodiment 1
500g, blue color 25g, HP-512 defoamers 5g.
The preparation method of above-mentioned bicomponent epoxy resin casting glue is：
A, the preparation process of component A
（1）In proportion precise E51 epoxy resin, butyl glycidyl ether, 1 Non-Gaussian Distribution aluminium hydrate powder of embodiment,
Blue color and HP-512 defoamer, then in order by E51 epoxy resin, butyl glycidyl ether, blue color and HP-
512 defoamers are added in reactor；
（2）Liquid components in reactor are stirred into 1 ± 0.5h of reaction at normal temperatures；
（3）By Non-Gaussian Distribution aluminium hydrate powder when preliminary drying 1 is small under the conditions of 90 ± 2 DEG C；
（4）Pre-baked Non-Gaussian Distribution aluminium hydrate powder is added in the liquid components that stir evenly, continue stirring 1.5 ±
0.5h；
（5）Reaction solution in reactor is transferred in vacuum defoaming device, deaeration 0.5h is left under the conditions of -0.1 ± 0.01MPa
The right side, that is, complete the preparation of component A；
B, when not in use, component A and B component separation storage, storage temperature are not higher than 40 DEG C；
C, when needing to use epoxy resin embedding adhesive, component A and B component is proportionally added into container at 25 DEG C and stirred
Vacuum defoamation after mixing, up to epoxy resin embedding adhesive；Gained casting glue can be at 25 DEG C in being used in 120min.
Embodiment 7
The preparation method of B component used in the present embodiment, the proportioning of component A and B component and component A with 6 phase of embodiment
Together, its composition difference difference lies in component A.
The component A is made of following component：
Commercially available bisphenol A type epoxy resin（E54）380g, diluent butyl glycidyl ether 100g, the Non-Gaussian Distribution of embodiment 1
Aluminium hydrate powder 490g, blue color 25g, HP-512 defoamers 5g.
Embodiment 8
The preparation method of B component used in the present embodiment, the proportioning of component A and B component and component A with 6 phase of embodiment
Together, its composition difference difference lies in component A.
The component A is made of following component：
Commercially available aliphatic epoxy resin 400g, diluent butyl glycidyl ether 39g, the Non-Gaussian Distribution hydroxide of embodiment 1
Aluminium powder 531g, blue color 25g, HP-512 defoamers 5g.
Embodiment 9
The preparation method of B component used in the present embodiment, the proportioning of component A and B component and component A with 6 phase of embodiment
Together, its composition difference difference lies in component A.
The component A is made of following component：
Commercially available cycloaliphatic epoxy resin 430g, diluent carbon lauryl diglycidyl ether 70g, the Non-Gaussian Distribution of embodiment 1
Aluminium hydrate powder 470g, blue color 25g, HP-512 defoamers 5g.
Embodiment 10
The preparation method of B component used in the present embodiment, the proportioning of component A and B component and component A with 6 phase of embodiment
Together, its composition difference difference lies in component A.
The component A is made of following component：
Commercially available bisphenol f type epoxy resin 460g, diluent benzyl glycidyl ether 80g, the Non-Gaussian Distribution hydroxide of embodiment 1
Aluminium powder 430g, blue color 25g, HP-512 defoamers 5g.
Epoxy resin embedding adhesive prepared by 6 ~ embodiment of Example 10 is tested for the property, and test method and test are tied
Fruit is shown in Table 2.
26 ~ embodiment of embodiment of table, 10 epoxy resin embedding adhesive performance data table
Note：Settlement test method is to take 200 grams of epoxy resin component A samples to enclose sample bottle, and 100h is stood at 80 DEG C, is seen
Whether examine has precipitation.
It can be seen that by the data of 6 ~ embodiment of embodiment 10 and regard Non-Gaussian Distribution aluminium hydrate powder as filler addition
In the component A of epoxy resin embedding adhesive casting glue, component A density can be reduced to below 3300cps, minimum is only 1300cps,
The mobility of component A is significantly strengthened；It can reach and do not precipitated in 100h at 80 DEG C at the same time, it was demonstrated that the homogeneity of component A is non-
Chang Hao, fully merge between each component, interact it is strong.
1 ~ comparative example of comparative example 3
The casting glue product component of the epoxy resin embedding adhesive of the comparative example and embodiment 6, proportioning, the basic phase of preparation method
Together, its difference lies in：
Comparative example 1 replaces embodiment Non-Gaussian Distribution aluminium hydrate powder with the aluminium hydrate powder that median is 8 μm；
Comparative example 2 replaces embodiment Non-Gaussian Distribution aluminium hydrate powder with the aluminium hydrate powder that median is 15 μm；
Comparative example 3 replaces embodiment Non-Gaussian Distribution aluminium hydrate powder with the aluminium hydrate powder that median is 25 μm.
Aluminium hydrate powder used in the 1 ~ comparative example of comparative example 3, is carried out using LS-POP (9) laser particle size analyzer
After particle diameter distribution, only obtain unimodal.For example, Fig. 2 is the aluminium hydrate powder particle diameter distribution that commercially available median is 8 μm
Figure, has significantly different with the bimodal particle size distribution figure in Fig. 1.
Example 6, the casting glue product of 1 ~ comparative example of comparative example 3 are tested for the property, test method and test result
It is shown in Table 3.
3 embodiment 6 of table, 1 ~ comparative example of comparative example, 3 epoxy resin embedding adhesive performance data table
Note：Settlement test method is to take 200 grams of epoxy resin component A samples to enclose sample bottle, and 100h is stood at 80 DEG C, is seen
Whether examine has precipitation.
It can be seen that by data in table 3 compared with the embodiment 6 using Non-Gaussian Distribution aluminium hydrate powder, comparative example
2nd, comparative example 3 is because the positive effect that aluminium hydrate powder particle diameter is larger and reduces component A viscosity, but can not meet that sedimentation is surveyed
The requirement of examination；And although comparative example 1 disclosure satisfy that the requirement of sedimentation test, and other specification differs not with the parameter of embodiment 6
Greatly, but its viscosity is higher by 1100mpas, the obvious use that is poor, can not meeting epoxy resin embedding adhesive of mobility compared with embodiment 6
Demand.
The above, is merely illustrative of the technical solution of the present invention and unrestricted, those of ordinary skill in the art are to this hair
The other modifications or equivalent substitution that bright technical solution is made, without departing from the spirit and scope of technical solution of the present invention,
It should all cover among scope of the presently claimed invention.
Claims (9)
- A kind of 1. Non-Gaussian Distribution aluminium hydrate powder, it is characterised in that：It it is 18 μm by aluminium hydrate powder and particle diameter that particle diameter is 2 μm Aluminium hydrate powder mix, both mixing quality ratios be 11：8~11：4.
- A kind of 2. Non-Gaussian Distribution aluminium hydrate powder according to claim 1, it is characterised in that：2 μm of aluminium hydroxide The mixing quality ratio of powder and 18 μm of aluminium hydrate powders is 11：7~11：5.
- 3. such as a kind of preparation method of Non-Gaussian Distribution aluminium hydrate powder of 1 or 2 any one of them of claim, it is characterised in that Comprise the steps of：A, crush：Aluminium hydroxide is crushed using original powder pulverizer, obtains the aluminium hydroxide of 2 μm and 18 μm two kinds of specifications Powder；B, screen：The aluminium hydrate powders of 2 μm and 18 μm is screened respectively with powder classification vibrating screen under room temperature, to ensure powder Body uniform particle diameter；C, mix：2 μm and 18 μm of aluminium hydrate powder is added in 360 ° of rotary blenders in mass ratio and is uniformly mixed, up to non- Normal distribution aluminium hydrate powder.
- A kind of 4. preparation method of Non-Gaussian Distribution aluminium hydrate powder according to claim 3, it is characterised in that：It is described mixed Close in step, mixing temperature is 90 ± 2 DEG C, and incorporation time is 2 ± 0.5h.
- 5. such as a kind of application of Non-Gaussian Distribution aluminium hydrate powder of 1 or 2 any one of them of claim, it is characterised in that：Institute State the preparation that Non-Gaussian Distribution aluminium hydrate powder is used for bicomponent epoxy resin electron pouring sealant as filler.
- A kind of 6. application of Non-Gaussian Distribution aluminium hydrate powder according to claim 5, it is characterised in that：The two-component The mass ratio of the component A and B component that epoxy resin electronic pouring sealant is preserved including separation, component A and B component is 100：20~25； The Non-Gaussian Distribution aluminium hydrate powder is added into component A as filler.
- A kind of 7. application of Non-Gaussian Distribution aluminium hydrate powder according to claim 6, it is characterised in that：The component A Include following component by weight percentage：Epoxy resin 35% ~ 50%, diluent 5% ~ 15%, Non-Gaussian Distribution aluminium hydroxide Powder 42% ~ 60%, color 1% ~ 5%, defoamer 0 ~ 1%；B component is polyamide curing agent.
- A kind of 8. application of Non-Gaussian Distribution aluminium hydrate powder according to claim 7, it is characterised in that：The component A Include following component by weight percentage：Epoxy resin 40% ~ 45%, diluent 5% ~ 8%, Non-Gaussian Distribution aluminium hydrate powder 45% ~ 50%, color 1% ~ 5%, defoamer 0 ~ 1%.
- 9. according to a kind of application of Non-Gaussian Distribution aluminium hydrate powder of 7 or 8 any one of them of claim, it is characterised in that： The epoxy resin is selected from bisphenol A type epoxy resin, bisphenol f type epoxy resin, cycloaliphatic epoxy resin, aliphatic epoxy resin In any one；The diluent is selected from butyl glycidyl ether, carbon lauryl diglycidyl ether benzyl glycidyl ether In any one；The defoamer is defoamer HP-512.
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