CN111334247A - Packaging adhesive for full-spectrum LED lamp - Google Patents
Packaging adhesive for full-spectrum LED lamp Download PDFInfo
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- CN111334247A CN111334247A CN202010304947.7A CN202010304947A CN111334247A CN 111334247 A CN111334247 A CN 111334247A CN 202010304947 A CN202010304947 A CN 202010304947A CN 111334247 A CN111334247 A CN 111334247A
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- packaging adhesive
- led lamp
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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
- C09J183/06—Polysiloxanes containing silicon bound to oxygen-containing groups
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G77/00—Macromolecular compounds obtained by reactions forming a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon in the main chain of the macromolecule
- C08G77/04—Polysiloxanes
- C08G77/14—Polysiloxanes containing silicon bound to oxygen-containing groups
- C08G77/18—Polysiloxanes containing silicon bound to oxygen-containing groups to alkoxy or aryloxy groups
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- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Organic Chemistry (AREA)
- Health & Medical Sciences (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Adhesives Or Adhesive Processes (AREA)
Abstract
The invention provides a packaging adhesive for a full-spectrum LED lamp. The organic silicon packaging adhesive prepared by the invention has the characteristics of high light transmittance, high refractive index, high thermal stability, high cohesiveness and the like, and is simple in preparation process, good in repeatability, controllable in product quality, low in impurity content of the product and suitable for industrial production.
Description
Technical Field
The invention belongs to the field of lighting materials, and particularly relates to a packaging adhesive for a full-spectrum LED lamp.
Background
Semiconductor lighting technology is one of the most promising high-tech fields in the 21 st century, and Light Emitting Diodes (LEDs) are the core technology. An LED is a light-emitting element that can directly convert electrical energy into light energy, and has a series of characteristics such as low operating voltage, low power consumption, high luminous efficiency, extremely short luminous response time, pure color, firm structure, impact resistance, vibration resistance, stable and reliable performance, light weight, small volume, and low cost. The LED lighting has the characteristics of small volume, high brightness and low energy consumption, is expected to replace incandescent lamps and fluorescent lamps to become mainstream indoor lighting sources, and therefore, the LED lighting is widely applied and developed rapidly.
In the structure of the LED light emitting body, besides the LED chip, the filling material is also one of the important factors for determining whether the LED light emitting body can be used for practical production and life. The potting adhesive is commonly used for heat conduction, bonding, sealing, potting, coating protection and the like of electronic components, and mainly has the effects of moisture protection, dust prevention, corrosion prevention, shock prevention, module stability improvement and the like. Especially, the appearance of white light high-power LED, because of its small volume, high power, high brightness and long service time, provides more rigorous optical and chemical performance requirements for the canned materials. The LED packaging adhesive has the advantages of color change resistance, high transparency, high temperature resistance and long service life, and is a preferred necessary condition of the LED packaging adhesive.
At present, the common high-power LED packaging adhesive is mainly composed of transparent bisphenol A type epoxy resin, but because the heat resistance, the color change resistance, the light transmission stability, the heat dissipation performance and other performances of the epoxy resin can not meet the performance indexes required by the existing high-power LED packaging, a more excellent material is required to be found to meet the requirement of the high-power LED packaging.
The most application of the epoxy resin pouring sealant is epoxy resin pouring sealant at present, and the biggest defects of the epoxy resin pouring sealant in application are poor heat conductivity and high viscosity, so that the service life of a device is shortened. In order to meet the market demand, it is necessary to modify the conventional epoxy resin potting adhesive in order to obtain a satisfactory encapsulation effect. In the research on epoxy resin pouring sealant for LED, bisphenol A epoxy resin is used as a main material, polyurethane is used as a toughening agent, and a mixed amine curing agent and an epoxy active diluent with low viscosity are used to prepare a product with low viscosity, good light transmittance and good mechanical property, but the modified epoxy pouring sealant has poor heat conduction effect and is not environment-friendly; ZnO in Al2O3Application research in heat-conducting epoxy resin pouring sealant, namely, in the text, the epoxy resin is modified by using the heat-conducting inorganic filler, so that the heat conductivity of the epoxy resin is improved to a certain extent, but the mechanical property of the epoxy resin is in a descending trend, and the viscosity of the epoxy resin is increased.
The organic silicon resin type packaging adhesive is developed in recent years, the existing organic silicon packaging adhesive is mainly formed by two-component addition type organic silicon resin, and the organic silicon resin has the advantages of high refractive index, good light transmission, color change resistance and the like. However, the organic silicon packaging adhesive has poor adhesive property and high temperature resistance, and the production cost is high. After the LED is packaged into a high-power LED, the service life of the LED is short.
The LED filament package mainly adopts methyl organic silicon system thixotrope with the refractive index of 1.41 at present. If a phenyl organosilicon system with the refractive index of about 1.53 is adopted, the refractive index difference between the packaging adhesive and the chip can be reduced, total reflection is reduced, and the light extraction efficiency is greatly improved. However, due to the structural limitation of the LED filament lamp, no heat radiation body is provided, and heat conduction can only be carried out by inert gas in the bulb, so that the working temperature of the LED filament is higher than that of other packaging forms, and the junction temperature of the 6w LED filament lamp can reach more than 120 ℃. The phenyl organosilicon system has high rigidity, so that the hardness of the phenyl organosilicon system is greatly increased and the toughness of the phenyl organosilicon system is deteriorated when the phenyl organosilicon system is operated at high temperature for a long time. The result that shows on the filament is that the packaging glue is just easy to split, and light then leads to the light efficiency to reduce, excessive blue light, and the heavy gold thread fracture appears dying the lamp. Therefore, there are also few reports on the application of phenyl silicones to LED filaments.
Therefore, development of a novel encapsulating material is urgently required.
Disclosure of Invention
The technical problem is as follows: in order to solve the defects of the prior art, the invention provides a packaging adhesive for a full-spectrum LED lamp.
The technical scheme is as follows: the invention provides a full-spectrum LED lamp packaging adhesive, which has the following structural formula:
the invention also provides a packaging adhesive for the full-spectrum LED lamp, which is prepared from the compound A, the compound B and the compound C, wherein,
The invention also provides a preparation method of the packaging adhesive for the full-spectrum LED lamp, which comprises the following steps:
(1) preparation of compound a: reacting hydrogen-containing silane and epoxy hexyl ethylene under the action of a Pt catalyst to obtain the catalyst;
(2) preparing packaging glue: adding the compound A, the compound B and the compound C into the monofunctional end capping agent compound D, and reacting under the action of a barium hydroxide catalyst to obtain the compound A;
the reaction formula is as follows:
in the step (1), the reaction temperature is 60-90 ℃ and the reaction time is 1-3 h.
And (2) specifically, uniformly mixing the compound A, the compound B, the compound C and the compound D to serve as reactants, adding distilled water and a barium hydroxide monohydrate catalyst, carrying out hydrolytic condensation reaction under the condition of heating and stirring, and carrying out pressure suction filtration after reaction to obtain the catalyst.
In the step (2), the reaction temperature is 60-90 ℃ and the reaction time is 2-4 h.
In the step (2), the mass ratio of reactants to distilled water is (1-3): 2.
has the advantages that: the organic silicon packaging adhesive prepared by the invention has the characteristics of high light transmittance, high refractive index, high thermal stability, high cohesiveness and the like, and is simple in preparation process, good in repeatability, controllable in product quality, low in impurity content of the product and suitable for industrial production.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1
The preparation method of the packaging adhesive for the full-spectrum LED lamp comprises the following steps:
(1) preparation of compound a: reacting hydrogen-containing silane and epoxy hexyl ethylene under the action of a Pt catalyst to obtain the catalyst; the reaction temperature is 75 ℃, and the reaction time is 2 h.
(2) Preparing packaging glue: uniformly mixing a compound A, a compound B, a compound C and a compound D to obtain a reactant, adding distilled water and a barium hydroxide monohydrate catalyst, heating to 75 ℃, and carrying out hydrolytic condensation reaction for 3 hours under the stirring condition, wherein the mass ratio of the reactant to the distilled water is 1: 1; and (4) after the reaction, pressurizing and filtering to obtain the catalyst.
Number average molecular weight 1120, weight average molecular weight 1690, molecular weight distribution index 1.468.
And (3) detecting the performance: the light transmittance is 93%, the refractive index at the temperature of 25 ℃ is 1.732, the thermogravimetric analysis result shows that the thermal decomposition temperature of the packaging adhesive is 469 ℃, the residual rate at the temperature of 700 ℃ is 72%, the packaging adhesive shows better heat resistance, the tensile strength and the elongation at break of the packaging adhesive are respectively 2.13MPa and 172%, and the Shore A hardness is 38.
Example 2
The preparation method of the packaging adhesive for the full-spectrum LED lamp comprises the following steps:
(1) preparation of compound a: reacting hydrogen-containing silane and epoxy hexyl ethylene under the action of a Pt catalyst to obtain the catalyst; the reaction temperature is 60 ℃, and the reaction time is 3 h.
(2) Preparing packaging glue: uniformly mixing a compound A, a compound B, a compound C and a compound D to obtain a reactant, adding distilled water and a barium hydroxide monohydrate catalyst, heating to 60 ℃, and carrying out hydrolytic condensation reaction for 4 hours under the stirring condition, wherein the mass ratio of the reactant to the distilled water is 1: 2; and (4) after the reaction, pressurizing and filtering to obtain the catalyst.
Number average molecular weight is 1140, weight average molecular weight is 1680, and molecular weight distribution index is 1.482.
And (3) detecting the performance: the light transmittance is 92%, the refractive index at the temperature of 25 ℃ is 1.692, the thermogravimetric analysis result shows that the thermal decomposition temperature of the packaging adhesive is 463 ℃, the residue rate at the temperature of 700 ℃ is 69%, the packaging adhesive shows better heat resistance, the tensile strength and the elongation at break of the packaging adhesive are 2.04MPa and 166%, respectively, and the Shore A hardness is 35.
Example 3
The preparation method of the packaging adhesive for the full-spectrum LED lamp comprises the following steps:
(1) preparation of compound a: reacting hydrogen-containing silane and epoxy hexyl ethylene under the action of a Pt catalyst to obtain the catalyst; the reaction temperature is 90 ℃ and the reaction time is 1 h.
(2) Preparing packaging glue: uniformly mixing a compound A, a compound B, a compound C and a compound D to obtain a reactant, adding distilled water and a barium hydroxide monohydrate catalyst, heating to 90 ℃, and carrying out hydrolysis condensation reaction for 2 hours under the stirring condition, wherein the mass ratio of the reactant to the distilled water is 3: 2; and (4) after the reaction, pressurizing and filtering to obtain the catalyst.
The number average molecular weight was 1150, the weight average molecular weight was 1710, and the molecular weight distribution index was 1.501.
And (3) detecting the performance: the light transmittance is 92%, the refractive index at the temperature of 25 ℃ is 1.687, the thermogravimetric analysis result shows that the thermal decomposition temperature of the packaging adhesive is 466 ℃, the residual rate at the temperature of 700 ℃ is 68%, the packaging adhesive shows better heat resistance, the tensile strength and the elongation at break of the packaging adhesive are respectively 2.07MPa and 169%, and the Shore A hardness is 34.
Furthermore, it should be understood that although the present description refers to embodiments, not every embodiment may contain only a single embodiment, and such description is for clarity only, and those skilled in the art should integrate the description, and the embodiments may be combined as appropriate to form other embodiments understood by those skilled in the art.
Claims (7)
2. the utility model provides a full gloss register for easy reference LED lamp is with encapsulation glue which characterized in that: prepared from a compound A, a compound B and a compound C,
wherein the content of the first and second substances,
3. The preparation method of the packaging adhesive for the full-spectrum LED lamp, as recited in claim 1, is characterized in that: the method comprises the following steps:
(1) preparation of compound a: reacting hydrogen-containing silane and epoxy hexyl ethylene under the action of a Pt catalyst to obtain the catalyst;
(2) preparing packaging glue: adding the compound A, the compound B and the compound C into the monofunctional end capping agent compound D, and reacting under the action of a barium hydroxide catalyst to obtain the compound A;
the reaction formula is as follows:
4. the method for preparing the packaging adhesive for the full-spectrum LED lamp according to claim 3, wherein the method comprises the following steps: in the step (1), the reaction temperature is 60-90 ℃ and the reaction time is 1-3 h.
5. The method for preparing the packaging adhesive for the full-spectrum LED lamp according to claim 3, wherein the method comprises the following steps: and (2) specifically, uniformly mixing the compound A, the compound B, the compound C and the compound D to serve as reactants, adding distilled water and a barium hydroxide monohydrate catalyst, carrying out hydrolytic condensation reaction under the condition of heating and stirring, and carrying out pressure suction filtration after reaction to obtain the catalyst.
6. The method for preparing the packaging adhesive for the full-spectrum LED lamp according to claim 3, wherein the method comprises the following steps: in the step (2), the reaction temperature is 60-90 ℃ and the reaction time is 2-4 h.
7. The method for preparing the packaging adhesive for the full-spectrum LED lamp according to claim 3, wherein the method comprises the following steps: in the step (2), the mass ratio of reactants to distilled water is (1-3): 2.
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CN202010304947.7A CN111334247A (en) | 2020-04-17 | 2020-04-17 | Packaging adhesive for full-spectrum LED lamp |
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Citations (5)
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---|---|---|---|---|
CN102807676A (en) * | 2012-08-16 | 2012-12-05 | 方舟(佛冈)化学材料有限公司 | Phenyl modified epoxy organic silicon resin and preparation method thereof, organic silicon packaging adhesive and LED lamp |
CN104745132A (en) * | 2015-03-17 | 2015-07-01 | 深圳市九晟光电通讯科技有限公司 | Epoxy resin adhesive for outdoor patch light beads and method for preparing epoxy resin adhesive for outdoor patch light beads |
CN106674523A (en) * | 2016-12-02 | 2017-05-17 | 华南理工大学 | Preparation method of methyl phenyl epoxy modified silicone oil for LED packaging |
CN109705352A (en) * | 2019-01-09 | 2019-05-03 | 杭州之江新材料有限公司 | A kind of vinyl polysiloxane and its preparation method and application |
CN109762167A (en) * | 2018-12-14 | 2019-05-17 | 中国科学院深圳先进技术研究院 | A kind of LED small-size chips heat conductive insulating die bond material and preparation method thereof |
-
2020
- 2020-04-17 CN CN202010304947.7A patent/CN111334247A/en not_active Withdrawn
Patent Citations (5)
Publication number | Priority date | Publication date | Assignee | Title |
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CN102807676A (en) * | 2012-08-16 | 2012-12-05 | 方舟(佛冈)化学材料有限公司 | Phenyl modified epoxy organic silicon resin and preparation method thereof, organic silicon packaging adhesive and LED lamp |
CN104745132A (en) * | 2015-03-17 | 2015-07-01 | 深圳市九晟光电通讯科技有限公司 | Epoxy resin adhesive for outdoor patch light beads and method for preparing epoxy resin adhesive for outdoor patch light beads |
CN106674523A (en) * | 2016-12-02 | 2017-05-17 | 华南理工大学 | Preparation method of methyl phenyl epoxy modified silicone oil for LED packaging |
CN109762167A (en) * | 2018-12-14 | 2019-05-17 | 中国科学院深圳先进技术研究院 | A kind of LED small-size chips heat conductive insulating die bond material and preparation method thereof |
CN109705352A (en) * | 2019-01-09 | 2019-05-03 | 杭州之江新材料有限公司 | A kind of vinyl polysiloxane and its preparation method and application |
Non-Patent Citations (2)
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汪洁 等: "《高折射率有机硅LED封装材料研究进展》", 《高分子通报》 * |
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