CN105754542B - Bi-component organic silicon casting glue and its preparation process - Google Patents
Bi-component organic silicon casting glue and its preparation process Download PDFInfo
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- CN105754542B CN105754542B CN201610112238.2A CN201610112238A CN105754542B CN 105754542 B CN105754542 B CN 105754542B CN 201610112238 A CN201610112238 A CN 201610112238A CN 105754542 B CN105754542 B CN 105754542B
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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
- C09J183/00—Adhesives based on macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon, with or without sulfur, nitrogen, oxygen, or carbon only; Adhesives based on derivatives of such polymers
- C09J183/04—Polysiloxanes
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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
- C09J11/02—Non-macromolecular additives
- C09J11/04—Non-macromolecular additives inorganic
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/02—Flame or fire retardant/resistant
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/22—Halogen free composition
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Abstract
The invention discloses its preparation processes of bi-component organic silicon casting glue machine, the bi-component organic silicon casting glue, including component A and B component: the component A is made of vinyl silicone oil, dimethicone, silicon powder, aluminium oxide, aluminium nitride, boron nitride, LSR base rubber, platinum catalyst by certain weight ratio mixing, and the B component is made of vinyl silicone oil, dimethicone, methyl hydrogen siloxane, silicon powder, aluminium oxide, LSR base rubber, white carbon black, tackifier, inhibitor by certain weight ratio mixing；The mixing ratio of the A component and B component is 1:1.The preparation process, comprises the following steps: (1) preparation of component A；(2) preparation of component B；(3) component A and component B is uniformly mixed under the action of high speed shear is dispersed by the mass ratio of 1:1, is placed in a vacuum drying oven vacuum defoamation 10 minutes, is subsequently poured into room temperature curing in mold or is heating and curing.
Description
Technical field
The present invention relates to a kind of two component more particularly to a kind of bi-component organic silicon casting glues.
Background technique
Organic silicon potting adhesive is due to excellent electrical insulation capability, high temperature resistance and ageing-resistant performance, goodization
Stability is learned, the advantages that processing technology is easy is widely used in electronics encapsulating field, plays moisture-proof, anticorrosion, shockproof, dust-proof
Effect, not only can be improved the service performance of electronic product, moreover it is possible to stablize the parameter of electronic component.But common organosilicon encapsulating
Glue there are thermal conductivities it is low, flame retardant property and adhesive property are poor the disadvantages of, seriously affected its application range.With present information skill
The development of art, electronic component, logic circuit tend to densification and miniaturization and the raising of appliance power, lead to electronic product unit
The heat of area is continuously increased, this proposes thermally conductive and fire-retardant new demand to organic silicon potting adhesive.At present generally by adding
Add a large amount of heat filling and inorganic fire retardants to prepare while have thermally conductive and anti-flammability organic silicon potting adhesive, so often
Cause physical mechanical property, mobility of casting glue etc. to decline, how to effectively improve the thermally conductive and flame retardant property of casting glue without
Being substantially reduced other performance is the difficult point studied at present.
At the same time, as the new generation of green light source and lighting engineering of environmental protection and energy saving, great power LED obtains fastly in recent years
Speed development.Great power LED still has the unsmooth and not high problem of light emission rate that radiates, because heat dissipation directly influences the reliable of LED
Property, and then influence its service life and application, and light emission rate is low directly constrains the development of LED, so being led to LED encapsulation material
It is hot, fire-retardant and out optical property research just seem increasingly important.
Summary of the invention
In view of the above-mentioned deficiencies in the prior art, the technical problem to be solved by the present invention is that it is organic to disclose two-component
Its preparation process of silicon casting glue machine, it is steady which maintains remaining performance while promoting thermally conductive and flame retardant property
It is fixed.
In order to achieve the above object, bi-component organic silicon casting glue of the invention, is achieved using following technical scheme:
Bi-component organic silicon casting glue, including component A and B component:
The component A by vinyl silicone oil, dimethicone, silicon powder, aluminium oxide, aluminium nitride, boron nitride, LSR base rubber,
Platinum catalyst is formed by certain weight ratio mixing,
The B component by vinyl silicone oil, dimethicone, methyl hydrogen siloxane, silicon powder, aluminium oxide, LSR base rubber,
White carbon black, tackifier, inhibitor are by certain weight ratio mixing composition；
The mixing ratio of the A component and B component is 1:1.
Further,
In the component A, vinyl silicone oil, dimethicone, silicon powder, aluminium oxide, aluminium nitride, boron nitride, LSR base
The weight ratio of glue, platinum catalyst are as follows: 100:(50~65): (20~30): (5~10): (5~10): (5~10): (20~30):
(0.5~3)；
In the B component, vinyl silicone oil, dimethicone, methyl hydrogen siloxane, silicon powder, aluminium oxide, LSR base rubber,
The weight ratio of white carbon black, tackifier, inhibitor are as follows: 100:(50~65): (20~30): (20~30): (5~10): (20~
30): (5~15): (0.1~1): (0.1~3)；
Further, in the component A using micron grade aluminum oxide, nanoscale aluminium nitride and boron nitride mixed fillers and
The shape of mixed fillers includes laminal filter, bat wool and ball filler；Mixed fillers described in the bat wool station
The 5~25% of total amount.
Moreover: the aluminium oxide, aluminium nitride and boron nitride are provided with there are many grain size specification；A variety of grains
Diameter specification is large, medium and small three kinds of grain size specifications；The mixed proportion of large, medium and small three kinds of grain size specifications is 10:30:15.
Further, the dosage of the platinum catalyst is less than 24ppm；The vinyl and methyl hydrogen of the vinyl silicone oil
The molar ratio of the silicon hydrogen-based of siloxanes is 1:(1~1.2).
Further, also including fire retardant；The fire retardant is halogen-free flame retardants；Halogen-free flame retardants be aluminium hydroxide,
One of magnesium hydroxide and zinc borate are a variety of；The halogen-free flame retardants by surface treatment, it is described surface treatment for via
Organosilicon processing.
Moreover: the fire retardant includes inorganic fire retardants and generates cooperateing with for synergistic effect with inorganic fire retardants
Fire retardant；The inorganic fire retardants is Strong oxdiative aluminium, and the synergistic fire retardant is platinum complex fire retardant.
The preparation process of bi-component organic silicon casting glue disclosed by the invention, comprises the following steps:
(1) preparation of component A；
Vinyl silicone oil, silicon powder, aluminium oxide, aluminium nitride and boron nitride high speed dispersion are mixed；High speed dispersion is mixed
Material afterwards is added in LSR base rubber and mixes with platinum catalyst, dimethicone, deaeration, solidifies up to component A；
(2) preparation of component B；
Vinyl silicone oil, dimethicone and aluminium oxide high speed dispersion are mixed；The mixed material of high speed dispersion is added
Enter in LSR base rubber and mixed with methyl hydrogen siloxane, silicon powder, tackifier, inhibitor and white carbon black, deaeration, solidified up to group
Part B；
(3) component A and component B is uniformly mixed under the action of high speed shear is dispersed by the mass ratio of 1:1, is placed in vacuum
Vacuum defoamation 10 minutes in drying box are subsequently poured into room temperature curing in mold or are heating and curing.
Further, the solidification temperature in the step (3) is 25~100 DEG C.
The medicine have the advantages that
In bi-component organic silicon glue casting glue of the invention, conductive filler material is multiple using aluminium oxide, aluminium nitride, boron nitride
The mode for closing filling, realizes organic silica gel maximum thermal conductivity.In addition, the present invention passes through specific matrix component and platinum catalysis
Agent can be realized a series of indexs such as the wide temperature range application of organic silica gel and flame retardant property, dielectric constant, linear shrinkage ratio, energy
Enough meet great power LED encapsulating application demand.
The present invention is also half reinforced filling using vinyl silicone oil, containing hydrogen silicone oil as crosslinking agent, silicon powder, is prepared for viscosity
It can good and excellent in mechanical performance after solidifying bi-component organic silicon casting glue.
Detailed description of the invention
Fig. 1 is the process flow chart of the component A of the preparation process of bi-component organic silicon casting glue of the invention；
Fig. 2 is the process flow chart of the component B of the preparation process of bi-component organic silicon casting glue of the invention.
Specific embodiment
Embodiments of the present invention are illustrated by particular specific embodiment below, those skilled in the art can be by this explanation
Content disclosed by book is understood other advantages and efficacy of the present invention easily.
The present invention improves existing two-component casting glue；The invention discloses a kind of more preferably bi-component organic silicons
Casting glue；Specific embodiment is as follows:
Embodiment 1:
Component A: vinyl silicone oil, dimethicone, silicon powder, aluminium oxide, aluminium nitride, boron nitride, LSR base rubber, platinum are urged
The weight ratio of agent are as follows: 100:60:25:8:8:8:25:2；
Component B: vinyl silicone oil, dimethicone, methyl hydrogen siloxane, silicon powder, aluminium oxide, LSR base rubber, hard charcoal
The weight ratio of black, tackifier, inhibitor are as follows: 100:60:25:25:8:25:10:0.5:2；
For component A: vinyl silicone oil, silicon powder, aluminium oxide, aluminium nitride and boron nitride high speed dispersion are mixed；It will be high
Material after fast dispersion mixing is added in LSR base rubber and mixes with platinum catalyst, dimethicone, deaeration, solidifies up to component
A；
For component B: vinyl silicone oil, dimethicone and aluminium oxide high speed dispersion are mixed；High speed dispersion is mixed
Rear material is added in LSR base rubber and mixes with methyl hydrogen siloxane, silicon powder, tackifier, inhibitor and white carbon black, deaeration,
Solidify up to component B；
Component A and component B is uniformly mixed under the action of high speed shear is dispersed by the mass ratio of 1:1, it is dry to be placed in vacuum
Vacuum defoamation 10 minutes in dry case are subsequently poured into room temperature curing in mold or are heating and curing.
Embodiment 2:
2 difference from Example 1 of embodiment is:
Component A: vinyl silicone oil, dimethicone, silicon powder, aluminium oxide, aluminium nitride, boron nitride, LSR base rubber, platinum are urged
The weight ratio of agent are as follows: 100:50:20:5:5:5:20:0.5；
Component B: vinyl silicone oil, dimethicone, methyl hydrogen siloxane, silicon powder, aluminium oxide, LSR base rubber, hard charcoal
The weight ratio of black, tackifier, inhibitor are as follows: 100:50:20:20:5:20:5:0.1:0.1.
Embodiment 3:
3 difference from Example 1 of embodiment is:
Component A: vinyl silicone oil, dimethicone, silicon powder, aluminium oxide, aluminium nitride, boron nitride, LSR base rubber, platinum are urged
The weight ratio of agent are as follows: 100:65:30:10:10:10:30:3；
Component B: vinyl silicone oil, dimethicone, methyl hydrogen siloxane, silicon powder, aluminium oxide, LSR base rubber, hard charcoal
The weight ratio of black, tackifier, inhibitor are as follows: 100:65:30:30:10:30:15:1:3.
For product made from Examples 1 to 3, We conducted measurements, obtain following result:
Curing time < 480min (25 DEG C), < 20min (80 DEG C)；
Thermal coefficient >=3.0W/mk；
Dielectric strength >=27kV/mm；
Dielectric constant 3.0~3.3 (1.2MHz)；
Volume resistivity >=1.0 × 1014 Ω cm (25 DEG C)；
Linear expansion coefficient≤2.2 × 10-4m/ (mK)
Therefore, the present invention has that thermal conductivity is big, and flame retardant property is good；Viscosity performance of the present invention is good and mechanical property after solidifying
It can be excellent；A series of indexs such as dielectric constant, linear shrinkage ratio can satisfy great power LED encapsulating application demand.
To sum up, a specific embodiment of the invention and preferred embodiment are as follows:
Bi-component organic silicon casting glue, including component A and B component:
The component A by vinyl silicone oil, dimethicone, silicon powder, aluminium oxide, aluminium nitride, boron nitride, LSR base rubber,
Platinum catalyst is formed by certain weight ratio mixing,
The B component by vinyl silicone oil, dimethicone, methyl hydrogen siloxane, silicon powder, aluminium oxide, LSR base rubber,
White carbon black, tackifier, inhibitor are by certain weight ratio mixing composition；
The mixing ratio of the A component and B component is 1:1.
In the component A, vinyl silicone oil, dimethicone, silicon powder, aluminium oxide, aluminium nitride, boron nitride, LSR base
The weight ratio of glue, platinum catalyst are as follows: 100:(50~65): (20~30): (5~10): (5~10): (5~10): (20~30):
(0.5~3)；
In the B component, vinyl silicone oil, dimethicone, methyl hydrogen siloxane, silicon powder, aluminium oxide, LSR base rubber,
The weight ratio of white carbon black, tackifier, inhibitor are as follows: 100:(50~65): (20~30): (20~30): (5~10): (20~
30): (5~15): (0.1~1): (0.1~3)；
It is preferred: micron grade aluminum oxide, nanoscale aluminium nitride and boron nitride mixed fillers and mixing are used in the component A
The shape of filler includes laminal filter, bat wool and ball filler；Mixed fillers total amount described in the bat wool station
5~25%.The machine silica gel glue of the present embodiment is using micron grade aluminum oxide, nanoscale aluminium nitride and boron nitride mixing filling
Mode, improve Embedding Material thermal conductivity to greatest extent in the case where guaranteeing colloid mobile performance.
Preferred: the aluminium oxide, aluminium nitride and boron nitride are provided with there are many grain size specification；A variety of grain size specifications
For large, medium and small three kinds of grain size specifications；The mixed proportion of large, medium and small three kinds of grain size specifications is 10:30:15.Using different-grain diameter, difference
Pattern, different types of heat filling fill casting glue by proper ratio, it is easier to obtain dense accumulation, be formed more thermally conductive
Access, therefore the organic silicon potting adhesive of high heat conductance can be prepared under lower loading.
Preferred: the dosage of the platinum catalyst is less than 24ppm；The vinyl and methyl hydrogen silicon oxygen of the vinyl silicone oil
The molar ratio of the silicon hydrogen-based of alkane is 1:(1~1.2).
It is preferred: also to include fire retardant；The fire retardant is halogen-free flame retardants；Halogen-free flame retardants is aluminium hydroxide, hydrogen-oxygen
Change one of magnesium and zinc borate or a variety of；The halogen-free flame retardants is by surface treatment, and the surface treatment is via organic
Silicon processing.
Preferred: the fire retardant includes inorganic fire retardants and generates the cooperative flame retardant of synergistic effect with inorganic fire retardants
Agent；The inorganic fire retardants is Strong oxdiative aluminium, and the synergistic fire retardant is platinum complex fire retardant.
Although the flame retardant property of halogen-free flameproof organic silicon potting adhesive can be improved in filling inorganic fire retardants, but can damage encapsulating
The physical mechanical property and mobility of glue.The present invention increases its phase with polymer by the surface treatment to inorganic fire retardants
Capacitive；The present invention also passes through synergistic fire retardant, cooperative flame retardant effect is generated with inorganic fire retardants, to reduce inorganic fire retardants
Dosage.
As shown, the preparation process of bi-component organic silicon casting glue disclosed by the invention, comprises the following steps:
(1) preparation of component A；
Vinyl silicone oil, silicon powder, aluminium oxide, aluminium nitride and boron nitride high speed dispersion are mixed；High speed dispersion is mixed
Material afterwards is added in LSR base rubber and mixes with platinum catalyst, dimethicone, deaeration, solidifies up to component A；
(2) preparation of component B；
Vinyl silicone oil, dimethicone and aluminium oxide high speed dispersion are mixed；The mixed material of high speed dispersion is added
Enter in LSR base rubber and mixed with methyl hydrogen siloxane, silicon powder, tackifier, inhibitor and white carbon black, deaeration, solidified up to group
Part B；
(3) component A and component B is uniformly mixed under the action of high speed shear is dispersed by the mass ratio of 1:1, is placed in vacuum
Vacuum defoamation 10 minutes in drying box are subsequently poured into room temperature curing in mold or are heating and curing.
Further, the solidification temperature in the step (3) is 25~100 DEG C.
Preparation process of the invention also includes the preparation of LSR base rubber, and the preparation of the LSR base rubber includes by vinyl silicone oil
With the process of silicon powder vacuum mixing 2h at 130 DEG C in kneader.
The preferred embodiment for the present invention is explained in detail above, but the present invention is not limited to the above embodiments,
Those of ordinary skill in the art within the scope of knowledge, can also make various without departing from the purpose of the present invention
Variation, these variations are related to the relevant technologies well-known to those skilled in the art, these both fall within the protection model of the invention patent
It encloses.
Many other changes and remodeling can be made by not departing from the spirit and scope of the present invention.It should be appreciated that the present invention is not
It is limited to specific embodiment, the scope of the present invention is defined by the following claims.
Claims (5)
1. bi-component organic silicon casting glue, including component A and B component, it is characterised in that:
The component A is urged by vinyl silicone oil, dimethicone, silicon powder, aluminium oxide, aluminium nitride, boron nitride, LSR base rubber, platinum
Agent is formed by certain weight ratio mixing,
The B component is by vinyl silicone oil, dimethicone, methyl hydrogen siloxane, silicon powder, aluminium oxide, LSR base rubber, hard charcoal
Black, tackifier, inhibitor are by certain weight ratio mixing composition；
The mixing ratio of the component A and B component is 1:1；
In the component A, vinyl silicone oil, dimethicone, silicon powder, aluminium oxide, aluminium nitride, boron nitride, LSR base rubber, platinum
The weight ratio of catalyst are as follows: 100:(50~65): (20~30): (5~10): (5~10): (5~10): (20~30): (0.5
~3)；
In the B component, vinyl silicone oil, dimethicone, methyl hydrogen siloxane, silicon powder, aluminium oxide, LSR base rubber, hard charcoal
The weight ratio of black, tackifier, inhibitor are as follows: 100:(50~65): (20~30): (20~30): (5~10): (20~30): (5
~15): (0.1~1): (0.1~3)；
The aluminium oxide, aluminium nitride and boron nitride are provided with there are many grain size specification；A variety of grain size specifications are large, medium and small three
Kind grain size specification；The mixed proportion of large, medium and small three kinds of grain size specifications is 10:30:15.
2. bi-component organic silicon casting glue as described in claim 1, it is characterised in that: use micron order oxygen in the component A
The shape for changing aluminium, nanoscale aluminium nitride and boron nitride mixed fillers and mixed fillers includes laminal filter, bat wool and ball
Shape filler；The bat wool accounts for the 5~25% of the mixed fillers total amount.
3. bi-component organic silicon casting glue as described in claim 1, it is characterised in that: the dosage of the platinum catalyst is less than
24ppm；The molar ratio of the silicon hydrogen-based of the vinyl and methyl hydrogen siloxane of the vinyl silicone oil is 1:(1~1.2).
4. bi-component organic silicon casting glue as described in claim 1, it is characterised in that: also include fire retardant；The fire retardant
For halogen-free flame retardants；Halogen-free flame retardants is one of aluminium hydroxide, magnesium hydroxide and zinc borate or a variety of；The halogen-free flameproof
Agent is to handle via organosilicon by surface treatment, the surface treatment.
5. bi-component organic silicon casting glue as claimed in claim 4, it is characterised in that: the fire retardant includes inorganic fire retardants
With the synergistic fire retardant for generating synergistic effect with inorganic fire retardants；The inorganic fire retardants is aluminium hydroxide, the cooperative flame retardant
Agent is platinum complex fire retardant.
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| CN106554625A (en) * | 2016-11-18 | 2017-04-05 | 石涛 | The preparation method and application of filling liquid, the filling liquid |
| CN107325782A (en) * | 2017-05-19 | 2017-11-07 | 天永诚高分子材料（常州）有限公司 | A kind of bi-component casting glue and preparation method thereof |
| CN107177345A (en) * | 2017-05-19 | 2017-09-19 | 天永诚高分子材料（常州）有限公司 | A kind of heat conduction Silica hydrogel and preparation method |
| CN107418506B (en) * | 2017-07-24 | 2021-02-19 | 东莞兆舜有机硅科技股份有限公司 | Organic silicon adhesive and use method and application thereof |
| CN109266009A (en) * | 2018-08-28 | 2019-01-25 | 厦门涛福精密机械有限公司 | A kind of moulding process vulcanizing contact arm |
| CN109337644B (en) * | 2018-09-30 | 2021-02-26 | 广州机械科学研究院有限公司 | Addition type room-temperature bonding two-component pouring sealant and preparation method thereof |
| CN110373151A (en) * | 2019-08-23 | 2019-10-25 | 深圳市红叶杰科技有限公司 | A kind of room temperature fast-curing wire and cable packaging silicon rubber and preparation method thereof |
| CN110699036B (en) * | 2019-10-17 | 2021-07-27 | 深圳天鼎新材料有限公司 | Pouring sealant and preparation method and application thereof |
| CN111394056B (en) * | 2020-04-09 | 2022-03-11 | 矽时代材料科技股份有限公司 | High-thermal-conductivity organic silicon gap filler |
| CN114350312B (en) * | 2022-01-27 | 2023-06-27 | 深圳诚立胜新材料科技有限公司 | High-temperature-resistant organic silicon composition and preparation method thereof |
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