CN105754542A - Two-component organic silicon pouring sealant and preparation process thereof - Google Patents
Two-component organic silicon pouring sealant and preparation process thereof Download PDFInfo
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- CN105754542A CN105754542A CN201610112238.2A CN201610112238A CN105754542A CN 105754542 A CN105754542 A CN 105754542A CN 201610112238 A CN201610112238 A CN 201610112238A CN 105754542 A CN105754542 A CN 105754542A
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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 a two-component organic silicon pouring sealant and a preparation process thereof. The two-component organic silicon pouring sealant comprises a component A and a component B, wherein the component A is prepared by mixing vinyl silicone oil, simethicone, silica powder, alumina, aluminum nitride, LSR base glue and a platinum catalyst in a certain weight ratio; and the component B is prepared by mixing vinyl silicone oil, simethicone, methyl hydrogen siloxane, silica powder, alumina, LSR base glue, white carbon black, a tackifier and an inhibitor in a certain weight ratio; and the mixing ratio of the component A and the component B is 1 to 1. The preparation process comprises the following steps: (1) preparing the component A; (2) preparing the component B; and (C) uniformly mixing the component A with the component B in a mass ratio of 1 to 1 under the high-speed shearing and dispersing, adding the mixture into a vacuum drying chamber, carrying out vacuum defoamation for 10 minutes, pouring the mixture into a mold, and curing at the room temperature or heating to cure.
Description
Technical field
The present invention relates to a kind of two component, particularly relate to a kind of bi-component organic silicon casting glue.
Background technology
Organic silicon potting adhesive is owing to having the electrical insulation capability of excellence, resistance to elevated temperatures and ageing-resistant performance, good chemical stability, the advantages such as processing technique is easy are widely used in electronics embedding field, play protection against the tide, anticorrosion, shockproof, dust-proof effect, it is possible not only to improve the serviceability of electronic product, moreover it is possible to stablize the parameter of electronic component.But the shortcomings such as common organic silicon potting adhesive exists, and thermal conductivity is low, fire resistance and adhesive property difference, have had a strong impact on its range of application.Along with the development of modern information technologies, electronic component, logic circuit tend to the raising of densification and miniaturization and appliance power, cause that the heat of electronic product unit are is continuously increased, and organic silicon potting adhesive is proposed heat conduction and fire-retardant new demand by this.The organic silicon potting adhesive with heat conduction and anti-flammability is prepared at present generally by the substantial amounts of heat filling of interpolation and inorganic combustion inhibitor, so often result in the physical and mechanical properties of casting glue, mobility etc. to decline, how to be effectively improved the heat conduction of casting glue and fire resistance and significantly reduce the difficult point that other performance is research at present.
Meanwhile, as new generation of green light source and the lighting engineering of environmental protection and energy saving, great power LED is rapidly developed in recent years.Great power LED remains in the problem that heat radiation is not smooth and light emission rate is not high, because heat radiation directly influences the reliability of LED, and then have influence on its life-span and application, and the low development directly constraining LED of light emission rate, so to the heat conduction of LED encapsulation material, fire-retardant and go out optical property research and just seem increasingly important.
Summary of the invention
The technical problem to be solved is in that for above-mentioned deficiency of the prior art, discloses bi-component organic silicon its preparation technology of casting glue machine, and this organic silicon potting adhesive has been maintained with all the other stable performances what promote heat conduction and fire resistance.
In order to achieve the above object, the bi-component organic silicon casting glue of the present invention, it is achieved by the following technical solutions:
Bi-component organic silicon casting glue, including component A and B component:
Described component A is made up of by certain weight ratio mixing vinyl silicone oil, dimethicone, silicon powder, aluminium oxide, aluminium nitride, boron nitride, LSR base glue, platinum catalyst,
Described B component is made up of by certain weight ratio mixing vinyl silicone oil, dimethicone, methyl hydrogen siloxane, silicon powder, aluminium oxide, LSR base glue, white carbon, viscosifier, inhibitor；
The mixing ratio of described A assembly and B assembly is 1:1.
Further:
In described component A, vinyl silicone oil, dimethicone, silicon powder, aluminium oxide, aluminium nitride, boron nitride, LSR base glue, platinum catalyst weight ratio be: 100:(50～65): (20～30): (5～10): (5～10): (5～10): (20～30): (0.5～3)；
In described B component, vinyl silicone oil, dimethicone, methyl hydrogen siloxane, silicon powder, aluminium oxide, LSR base glue, white carbon, viscosifier, inhibitor weight ratio be: 100:(50～65): (20～30): (20～30): (5～10): (20～30): (5～15): (0.1～1): (0.1～3)；
Further: described component A adopts the shape of micron order aluminium oxide, nanoscale aluminium nitride and boron nitride mixed fillers and mixed fillers comprise laminal filter, bat wool and ball filler；Described in described bat wool station the 5～25% of mixed fillers total amount.
Moreover: described aluminium oxide, aluminium nitride and boron nitride have been provided with multiple grain size specification；Described multiple grain size specification is large, medium and small three kinds of grain size specification；The mixed proportion of large, medium and small three kinds of grain size specification is 10:30:15.
Further: the consumption of described platinum catalyst is less than 24ppm；The mol ratio of the silicon hydrogen-based of the vinyl of described vinyl silicone oil and methyl hydrogen siloxane is 1:(1～1.2).
Further: also comprise fire retardant；Described fire retardant is halogen-free flame retardants；Halogen-free flame retardants is one or more in aluminium hydroxide, magnesium hydroxide and Firebrake ZB；Described halogen-free flame retardants passes through surface treatment, and described surface treatment is process via organosilicon.
Moreover: described fire retardant comprises inorganic combustion inhibitor and produces synergistic synergistic fire retardant with inorganic combustion inhibitor；Described inorganic combustion inhibitor is Strong oxdiative aluminum, and described synergistic fire retardant is platinum complex fire retardant.
The preparation technology of bi-component organic silicon casting glue disclosed by the invention, comprises the steps of:
(1) preparation of component A；
Vinyl silicone oil, silicon powder, aluminium oxide, aluminium nitride and boron nitride high speed dispersion are mixed；Added by mixed for high speed dispersion material in LSR base glue and mix with platinum catalyst, dimethicone, namely deaeration, solidification obtain component A；
(2) preparation of component B；
Vinyl silicone oil, dimethicone and aluminium oxide high speed dispersion are mixed；Added by mixed for high speed dispersion material in LSR base glue and mix with methyl hydrogen siloxane, silicon powder, viscosifier, inhibitor and white carbon, namely deaeration, solidification obtain component B；
(3) component A and component B is pressed mass ratio mix homogeneously under the scattered effect of high speed shear of 1:1, is placed in vacuum drying oven vacuum defoamation 10 minutes, be subsequently poured in mould cold curing or be heating and curing.
Further: the solidification temperature in described step (3) is 25～100 DEG C.
The medicine have the advantages that
In the bi-component organic silicon glue casting glue of the present invention, conductive filler material adopts the mode that aluminium oxide, aluminium nitride, boron nitride are composite filled, it is achieved that the maximum thermal conductivity of organic silica gel.It addition, the present invention is by concrete matrix component and platinum catalyst, it is possible to realize a series of indexs such as the application of organic silica gel width temperature range and fire resistance, dielectric constant, linear shrinkage ratio, it is possible to meet great power LED embedding application demand.
The present invention also with vinyl silicone oil, containing hydrogen silicone oil be cross-linking agent, silicon powder be half reinforced filling, be prepared for good and excellent in mechanical performance after solidifying the bi-component organic silicon casting glue of viscosity performance.
Accompanying drawing explanation
Fig. 1 is the process chart of the component A of the preparation technology of the bi-component organic silicon casting glue of the present invention；
Fig. 2 is the process chart of the component B of the preparation technology of the bi-component organic silicon casting glue of the present invention.
Detailed description of the invention
By particular specific embodiment, embodiments of the present invention being described below, those skilled in the art the content disclosed by this specification can understand other advantages and effect of the present invention easily.
Existing double-component casting glue has been improved by the present invention；The invention discloses a kind of more excellent bi-component organic silicon 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 glue, platinum catalyst weight ratio be: 100:60:25:8:8:8:25:2；
Component B: vinyl silicone oil, dimethicone, methyl hydrogen siloxane, silicon powder, aluminium oxide, LSR base glue, white carbon, viscosifier, inhibitor weight ratio be: 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；Added by mixed for high speed dispersion material in LSR base glue and mix with platinum catalyst, dimethicone, namely deaeration, solidification obtain component A；
For component B: vinyl silicone oil, dimethicone and aluminium oxide high speed dispersion are mixed；Added by mixed for high speed dispersion material in LSR base glue and mix with methyl hydrogen siloxane, silicon powder, viscosifier, inhibitor and white carbon, namely deaeration, solidification obtain component B；
Component A and component B is pressed mass ratio mix homogeneously under the scattered effect of high speed shear of 1:1, is placed in vacuum drying oven vacuum defoamation 10 minutes, be subsequently poured in mould cold curing or be heating and curing.
Embodiment 2:
Embodiment 2 difference from Example 1 is in that:
Component A: vinyl silicone oil, dimethicone, silicon powder, aluminium oxide, aluminium nitride, boron nitride, LSR base glue, platinum catalyst weight ratio be: 100:50:20:5:5:5:20:0.5；
Component B: vinyl silicone oil, dimethicone, methyl hydrogen siloxane, silicon powder, aluminium oxide, LSR base glue, white carbon, viscosifier, inhibitor weight ratio be: 100:50:20:20:5:20:5:0.1:0.1.
Embodiment 3:
Embodiment 3 difference from Example 1 is in that:
Component A: vinyl silicone oil, dimethicone, silicon powder, aluminium oxide, aluminium nitride, boron nitride, LSR base glue, platinum catalyst weight ratio be: 100:65:30:10:10:10:30:3；
Component B: vinyl silicone oil, dimethicone, methyl hydrogen siloxane, silicon powder, aluminium oxide, LSR base glue, white carbon, viscosifier, inhibitor weight ratio be: 100:65:30:30:10:30:15:1:3.
For the product that embodiment 1～3 prepares, We conducted measurement, draw following result:
Hardening time < 480min (25 DEG C), < 20min (80 DEG C)；
Heat conductivity >=3.0W/m k；
Dielectric strength >=27kV/mm；
Dielectric constant 3.0～3.3 (1.2MHz)；
Specific insulation >=1.0 × 1014 Ω cm (25 DEG C)；
Linear expansion coefficient≤2.2 × 10-4m/ (m K)
Therefore, it is big that the present invention possesses thermal conductivity, and fire resistance is good；Viscosity performance of the present invention is good and excellent in mechanical performance after solidifying；A series of index such as dielectric constant, linear shrinkage ratio disclosure satisfy that great power LED embedding application demand.
To sum up, the specific embodiment of the present invention and preferred implementation are as follows:
Bi-component organic silicon casting glue, including component A and B component:
Described component A is made up of by certain weight ratio mixing vinyl silicone oil, dimethicone, silicon powder, aluminium oxide, aluminium nitride, boron nitride, LSR base glue, platinum catalyst,
Described B component is made up of by certain weight ratio mixing vinyl silicone oil, dimethicone, methyl hydrogen siloxane, silicon powder, aluminium oxide, LSR base glue, white carbon, viscosifier, inhibitor；
The mixing ratio of described A assembly and B assembly is 1:1.
In described component A, vinyl silicone oil, dimethicone, silicon powder, aluminium oxide, aluminium nitride, boron nitride, LSR base glue, platinum catalyst weight ratio be: 100:(50～65): (20～30): (5～10): (5～10): (5～10): (20～30): (0.5～3)；
In described B component, vinyl silicone oil, dimethicone, methyl hydrogen siloxane, silicon powder, aluminium oxide, LSR base glue, white carbon, viscosifier, inhibitor weight ratio be: 100:(50～65): (20～30): (20～30): (5～10): (20～30): (5～15): (0.1～1): (0.1～3)；
Preferred: described component A to adopt the shape of micron order aluminium oxide, nanoscale aluminium nitride and boron nitride mixed fillers and mixed fillers comprise laminal filter, bat wool and ball filler；Described in described bat wool station the 5～25% of mixed fillers total amount.The machine silica gel glue of the present embodiment adopts the mode that micron order aluminium oxide, nanoscale aluminium nitride and boron nitride mixing are filled, and improves Embedding Material thermal conductivity to greatest extent when ensureing colloid mobile performance.
Preferred: described aluminium oxide, aluminium nitride and boron nitride have been provided with multiple grain size specification；Described multiple grain size specification is large, medium and small three kinds of grain size specification；The mixed proportion of large, medium and small three kinds of grain size specification is 10:30:15.Adopt different-grain diameter, different-shape, different types of heat filling to fill casting glue by proper ratio, it is easier to obtain dense accumulation, form more thermal conducting path, the organic silicon potting adhesive of high heat conductance therefore under relatively low loading, can be prepared.
Preferred: the consumption of described platinum catalyst is less than 24ppm；The mol ratio of the silicon hydrogen-based of the vinyl of described vinyl silicone oil and methyl hydrogen siloxane is 1:(1～1.2).
Preferred: also to comprise fire retardant；Described fire retardant is halogen-free flame retardants；Halogen-free flame retardants is one or more in aluminium hydroxide, magnesium hydroxide and Firebrake ZB；Described halogen-free flame retardants passes through surface treatment, and described surface treatment is process via organosilicon.
Preferred: described fire retardant comprises inorganic combustion inhibitor and produces synergistic synergistic fire retardant with inorganic combustion inhibitor；Described inorganic combustion inhibitor is Strong oxdiative aluminum, and described synergistic fire retardant is platinum complex fire retardant.
Although filling inorganic combustion inhibitor can improve the fire resistance of halogen-free flameproof organic silicon potting adhesive, but physical and mechanical properties and the mobility of casting glue can be damaged.The present invention, by the surface treatment to inorganic combustion inhibitor, increases the compatibility of itself and polymer；The present invention, also by synergistic fire retardant, produces cooperative flame retardant effect with inorganic combustion inhibitor, thus reducing the consumption of inorganic combustion inhibitor.
As it can be seen, the preparation technology of bi-component organic silicon casting glue disclosed by the invention, comprise the steps of:
(1) preparation of component A；
Vinyl silicone oil, silicon powder, aluminium oxide, aluminium nitride and boron nitride high speed dispersion are mixed；Added by mixed for high speed dispersion material in LSR base glue and mix with platinum catalyst, dimethicone, namely deaeration, solidification obtain component A；
(2) preparation of component B；
Vinyl silicone oil, dimethicone and aluminium oxide high speed dispersion are mixed；Added by mixed for high speed dispersion material in LSR base glue and mix with methyl hydrogen siloxane, silicon powder, viscosifier, inhibitor and white carbon, namely deaeration, solidification obtain component B；
(3) component A and component B is pressed mass ratio mix homogeneously under the scattered effect of high speed shear of 1:1, is placed in vacuum drying oven vacuum defoamation 10 minutes, be subsequently poured in mould cold curing or be heating and curing.
Further: the solidification temperature in described step (3) is 25～100 DEG C.
The preparation technology of the present invention also comprises the preparation of LSR base glue, and the preparation of described LSR base glue comprises vinyl silicone oil and the silicon powder process of vacuum mixing 2h at 130 DEG C in kneader.
Above the preferred embodiment for the present invention is explained in detail; but the invention is not restricted to above-mentioned embodiment; in the ken that those of ordinary skill in the art possess; can also make a variety of changes under the premise without departing from present inventive concept; these changes relate to correlation technique well-known to those skilled in the art, and these both fall within the protection domain of patent of the present invention.
Many other can be made without departing from the spirit and scope of the present invention to change and remodeling.Should be appreciated that and the invention is not restricted to specific embodiment, the scope of the invention limits.
Claims (9)
1. bi-component organic silicon casting glue, including component A and B component, it is characterised in that:
Described component A is made up of by certain weight ratio mixing vinyl silicone oil, dimethicone, silicon powder, aluminium oxide, aluminium nitride, boron nitride, LSR base glue, platinum catalyst,
Described B component is made up of by certain weight ratio mixing vinyl silicone oil, dimethicone, methyl hydrogen siloxane, silicon powder, aluminium oxide, LSR base glue, white carbon, viscosifier, inhibitor；
The mixing ratio of described A assembly and B assembly is 1:1.
2. bi-component organic silicon casting glue as claimed in claim 1, it is characterised in that:
In described component A, vinyl silicone oil, dimethicone, silicon powder, aluminium oxide, aluminium nitride, boron nitride, LSR base glue, platinum catalyst weight ratio be: 100:(50～65): (20～30): (5～10): (5～10): (5～10): (20～30): (0.5～3)；
In described B component, vinyl silicone oil, dimethicone, methyl hydrogen siloxane, silicon powder, aluminium oxide, LSR base glue, white carbon, viscosifier, inhibitor weight ratio be: 100:(50～65): (20～30): (20～30): (5～10): (20～30): (5～15): (0.1～1): (0.1～3).
3. bi-component organic silicon casting glue as claimed in claim 2, it is characterised in that: described component A adopt the shape of micron order aluminium oxide, nanoscale aluminium nitride and boron nitride mixed fillers and mixed fillers comprise laminal filter, bat wool and ball filler；Described in described bat wool station the 5～25% of mixed fillers total amount.
4. bi-component organic silicon casting glue as claimed in claim 3, it is characterised in that: described aluminium oxide, aluminium nitride and boron nitride have been provided with multiple grain size specification；Described multiple grain size specification is large, medium and small three kinds of grain size specification；The mixed proportion of large, medium and small three kinds of grain size specification is 10:30:15.
5. bi-component organic silicon casting glue as claimed in claim 2, it is characterised in that: the consumption of described platinum catalyst is less than 24ppm；The mol ratio of the silicon hydrogen-based of the vinyl of described vinyl silicone oil and methyl hydrogen siloxane is 1:(1～1.2).
6. bi-component organic silicon casting glue as claimed in claim 2, it is characterised in that: also comprise fire retardant；Described fire retardant is halogen-free flame retardants；Halogen-free flame retardants is one or more in aluminium hydroxide, magnesium hydroxide and Firebrake ZB；Described halogen-free flame retardants passes through surface treatment, and described surface treatment is process via organosilicon.
7. bi-component organic silicon casting glue as claimed in claim 6, it is characterised in that: described fire retardant comprises inorganic combustion inhibitor and produces synergistic synergistic fire retardant with inorganic combustion inhibitor；Described inorganic combustion inhibitor is Strong oxdiative aluminum, and described synergistic fire retardant is platinum complex fire retardant.
8. the preparation technology of bi-component organic silicon casting glue, comprises the steps of:
(1) preparation of component A；
Vinyl silicone oil, silicon powder, aluminium oxide, aluminium nitride and boron nitride high speed dispersion are mixed；Added by mixed for high speed dispersion material in LSR base glue and mix with platinum catalyst, dimethicone, namely deaeration, solidification obtain component A；
(2) preparation of component B；
Vinyl silicone oil, dimethicone and aluminium oxide high speed dispersion are mixed；Added by mixed for high speed dispersion material in LSR base glue and mix with methyl hydrogen siloxane, silicon powder, viscosifier, inhibitor and white carbon, namely deaeration, solidification obtain component B；
(3) component A and component B is pressed mass ratio mix homogeneously under the scattered effect of high speed shear of 1:1, is placed in vacuum drying oven vacuum defoamation 10 minutes, be subsequently poured in mould cold curing or be heating and curing.
9. the preparation technology of bi-component organic silicon casting glue as claimed in claim 8, it is characterised in that: the solidification temperature in described step (3) is 25～100 DEG C.
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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 |
| 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 |
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| CN109337644A (en) * | 2018-09-30 | 2019-02-15 | 广州机械科学研究院有限公司 | A kind of add-on type room temperature two-component casting glue 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 |
| CN110699036A (en) * | 2019-10-17 | 2020-01-17 | 深圳天鼎新材料有限公司 | Pouring sealant and preparation method and application 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 |
| CN111394056A (en) * | 2020-04-09 | 2020-07-10 | 矽时代材料科技股份有限公司 | High-thermal-conductivity organic silicon gap filler |
| 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 |
| CN114350312A (en) * | 2022-01-27 | 2022-04-15 | 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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| CN105754542B (en) | 2019-06-11 |
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Denomination of invention: Two component silicone potting adhesive and its preparation process Effective date of registration: 20210714 Granted publication date: 20190611 Pledgee: Shenzhen hi tech investment small loan Co.,Ltd. Pledgor: SHENZHEN EVOPUTE INDUSTRY MATERIAL Co.,Ltd. Registration number: Y2021980006111 |
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