CN105112006A - Ketoxime-removal organosilicon sealant for LED (light-emitting diode) packaging and preparation method thereof - Google Patents

Abstract

The invention relates to a deketoxime type silicone sealant for LED packaging and a preparation method thereof, belonging to the technical field of silicone sealants. The silicone sealant of the present invention comprises: 80-100 parts of hydroxyl-terminated polydimethylsiloxane, 15-25 parts of crosslinking agent methyltributanone oxime silane, and 5-15 parts of crosslinking agent phenyltrimethoxysilane , stannous octoate 0.5-5 parts, KH-570? 1.5-2.5 parts, KH-792? 1.5-2.5 parts, dispersant 2-4 parts, pigment chromium oxide 5-9 parts, barium sulfate 30-38 parts, light 30-36 parts of calcium carbonate. The present invention adopts methyl tributanone oxime silane as the main crosslinking agent and adds a small amount of dealcoholization crosslinking agent phenyltrimethoxysilane to form a mixed crosslinking system, and prepares a comprehensive mechanical One-component ketoxime type silicone sealant with better performance, very suitable for LED packaging.

Description

A kind of deketoxime type silicone sealant for LED packaging and preparation method thereof

technical field

The invention relates to a silicone sealant and a preparation method thereof. More specifically, the invention relates to a deketoxime type silicone sealant for LED packaging and a preparation method thereof, belonging to the technical field of silicone sealants.

Background technique

One-component room temperature vulcanized silicone sealant refers to mixing room temperature vulcanized silicone rubber and fillers, adding crosslinking agents, catalysts and other components, and under the condition of complete dehydration in a single-component form of airtight packaging, use and Storage, a type of silicone sealant product that can be cured into an elastomer by absorbing moisture in the air. According to the types of small molecules removed during condensation, they can be divided into deacetic acid type, deketoxime type, acetone type, deamidation type, deamination type and dealcoholization type. Deketoxime type silicone sealant is widely used because of its good bonding performance, fast curing speed, low odor, and less corrosion than acetic acid type and amine type.

The State Intellectual Property Office disclosed an invention with the publication number CN101935455A titled "A Silicone Material for LED Packaging and Its Preparation Method" on January 5, 2011. The silicone material of this invention is characterized in that it is composed of A component Vinyl polysiloxane, component B is hydrogen-containing polysiloxane, mixed according to the mass ratio of 0.3:1~1:30, then add component D vinyl MQ resin, component E is vinyl trimethoxysilane , n-butyl titanate, KH-560 and a mixture of one or more of them and the catalyst C component are prepared after uniform mixing. Another technical problem to be solved by the present invention is to make the preparation method clean and pollution-free. In the preparation method of the present invention, after mixing the components evenly according to the proportion, vacuum degassing at room temperature for 5-30 minutes, and the vulcanization temperature is 20-150 ° C. Vulcanization molding.

The above-mentioned organosilicon materials used for LED packaging have poor comprehensive properties.

Contents of the invention

The invention aims to solve the problem of organic silicon materials for LED packaging in the prior art, and provides a deketoxime type silicone sealant for LED packaging. The sealant machine has good comprehensive performance and is very suitable for LED potting.

In order to realize the above-mentioned purpose of the invention, its concrete technical scheme is as follows:

A deketoxime type silicone sealant for LED packaging, characterized in that: it comprises the following raw materials in parts by weight:

80-100 parts of hydroxyl-terminated polydimethylsiloxane

15-25 parts of crosslinking agent methyl tributanone oxime silane

5-15 parts of crosslinking agent phenyltrimethoxysilane

0.5-5 parts of stannous octoate

KH-570 1.5-2.5 copies

KH-7921.5-2.5 parts

2-4 parts of dispersant

Pigment chromium oxide 5-9 parts

30-38 parts of barium sulfate

30-36 parts of light calcium carbonate.

The viscosity of the hydroxyl-terminated polydimethylsiloxane of the present invention is 15000-20000 mPa·s.

The dispersant of the present invention is orthophosphate.

A method for preparing a deketoxime type silicone sealant for LED packaging, characterized in that it comprises the following process steps:

A. First mix the hydroxyl-terminated polydimethylsiloxane with dispersant, pigment chromium oxide, barium sulfate and light calcium carbonate in a kneader;

B. Raise the temperature to 135-145°C, knead and stir in vacuum for 2-3h;

C. Vacuum dehydration for 2-3 hours, lower the temperature to room temperature, grind evenly in a three-roll mill, and discharge to obtain base rubber;

D. Add base glue, KH-570, KH-792 into the high-speed mixer;

E. Vacuum dehydration for 2-3 hours, add cross-linking agent methyl tributanone oxime silane, cross-linking agent phenyltrimethoxysilane, mix well;

F. Add the catalyst stannous octoate and mix well, defoam; discharge and pack.

Beneficial technical effects brought by the present invention:

The invention solves the problem of poor comprehensive performance of organic silicon materials used for LED packaging. The present invention adopts methyl tributanone oxime silane as the main crosslinking agent and adds a small amount of dealcoholization crosslinking agent phenyltrimethoxysilane to form a mixed crosslinking system, and prepares a comprehensive mechanical One-component ketoxime type silicone sealant with better performance, very suitable for LED packaging.

Detailed ways

Example 1

A deketoxime type silicone sealant for LED packaging, comprising the following raw materials in parts by weight:

80 parts of hydroxyl-terminated polydimethylsiloxane

15 parts of crosslinking agent methyl tributanone oxime silane

5 parts of crosslinking agent phenyltrimethoxysilane

0.5 parts of stannous octoate

KH-5701.5 parts

KH-7921.5 copies

Dispersant 2 parts

Pigment chromium oxide 5 parts

Barium sulfate 30 parts

30 parts of light calcium carbonate.

Example 2

A deketoxime type silicone sealant for LED packaging, comprising the following raw materials in parts by weight:

100 parts of hydroxyl-terminated polydimethylsiloxane

25 parts of crosslinking agent methyl tributanone oxime silane

15 parts of crosslinking agent phenyltrimethoxysilane

5 parts stannous octoate

KH-570 2.5 copies

KH-7922.5 copies

4 parts of dispersant

Pigment chromium oxide 9 parts

Barium sulfate 38 parts

36 parts of light calcium carbonate.

Example 3

A deketoxime type silicone sealant for LED packaging, comprising the following raw materials in parts by weight:

90 parts of hydroxyl-terminated polydimethylsiloxane

20 parts of crosslinking agent methyl tributanone oxime silane

10 parts of crosslinking agent phenyltrimethoxysilane

Stannous octoate 2.75 parts

KH-5702 copies

KH-7922 copies

3 parts of dispersant

Pigment chromium oxide 7 parts

Barium sulfate 34 parts

33 parts of light calcium carbonate.

Example 4

A deketoxime type silicone sealant for LED packaging, comprising the following raw materials in parts by weight:

95 parts of hydroxyl-terminated polydimethylsiloxane

21 parts of crosslinking agent methyl tributanone oxime silane

7 parts of crosslinking agent phenyltrimethoxysilane

Stannous octoate 1.5 parts

KH-570 2.1 copies

KH-7921.8 copies

3.6 parts of dispersant

Pigment chromium oxide 8 parts

Barium sulfate 35 parts

35 parts of light calcium carbonate.

Example 5

On the basis of embodiment 1-4:

Preferably, the viscosity of the hydroxyl-terminated polydimethylsiloxane is 15000 mPa·s.

Preferably, the dispersant is orthophosphate.

Example 6

On the basis of embodiment 1-4:

Preferably, the viscosity of the hydroxyl-terminated polydimethylsiloxane is 20000 mPa·s.

Preferably, the dispersant is orthophosphate.

Example 7

On the basis of embodiment 1-4:

Preferably, the viscosity of the hydroxyl-terminated polydimethylsiloxane is 17500 mPa·s.

Preferably, the dispersant is orthophosphate.

Example 8

On the basis of embodiment 1-4:

Preferably, the viscosity of the hydroxyl-terminated polydimethylsiloxane is 16000 mPa·s.

Preferably, the dispersant is orthophosphate.

Example 9

A preparation method for deketoxime type silicone sealant for LED encapsulation, comprising the following process steps:

A. First mix the hydroxyl-terminated polydimethylsiloxane with dispersant, pigment chromium oxide, barium sulfate and light calcium carbonate in a kneader;

B. Raise the temperature to 135°C, knead and stir in vacuum for 2 hours;

C. Vacuum dehydration for 2 hours, lower the temperature to room temperature, grind evenly in a three-roll mill, and discharge to obtain base glue;

D. Add base glue, KH-570, KH-792 into the high-speed mixer;

E. Vacuum dehydration for 2 hours, add cross-linking agent methyl tributanone oxime silane, cross-linking agent phenyltrimethoxysilane, mix well;

F. Add the catalyst stannous octoate and mix well, defoam; discharge and pack.

Example 10

A preparation method for deketoxime type silicone sealant for LED encapsulation, comprising the following process steps:

A. First mix the hydroxyl-terminated polydimethylsiloxane with dispersant, pigment chromium oxide, barium sulfate and light calcium carbonate in a kneader;

B. Raise the temperature to 145°C, knead and stir in vacuum for 3 hours;

C. Vacuum dehydration for 3 hours, lower the temperature to room temperature, grind evenly in a three-roll mill, and discharge to obtain base rubber;

D. Add base glue, KH-570, KH-792 into the high-speed mixer;

E. Vacuum dehydration for 3 hours, add cross-linking agent methyl tributanone oxime silane, cross-linking agent phenyltrimethoxysilane, and mix well;

F. Add the catalyst stannous octoate and mix well, defoam; discharge and pack.

Example 11

A preparation method for deketoxime type silicone sealant for LED encapsulation, comprising the following process steps:

A. First mix the hydroxyl-terminated polydimethylsiloxane with dispersant, pigment chromium oxide, barium sulfate and light calcium carbonate in a kneader;

B. Raise the temperature to 140°C, knead and stir in vacuum for 2.5 hours;

C. Vacuum dehydration for 2.5 hours, lower the temperature to room temperature, grind evenly in a three-roll mill, and discharge to obtain base rubber;

D. Add base glue, KH-570, KH-792 into the high-speed mixer;

E. Vacuum dehydration for 2.5 hours, add cross-linking agent methyl tributanone oxime silane, cross-linking agent phenyltrimethoxysilane, mix well;

F. Add the catalyst stannous octoate and mix well, defoam; discharge and pack.

Example 12

A preparation method for deketoxime type silicone sealant for LED encapsulation, comprising the following process steps:

A. First mix the hydroxyl-terminated polydimethylsiloxane with dispersant, pigment chromium oxide, barium sulfate and light calcium carbonate in a kneader;

B. Raise the temperature to 138°C, knead and stir in vacuum for 2.25h;

C. Vacuum dehydration for 2.25 hours, lower the temperature to room temperature, grind evenly in a three-roll mill, and discharge to obtain base glue;

D. Add base glue, KH-570, KH-792 into the high-speed mixer;

E. Vacuum dehydration for 2.75h, add cross-linking agent methyl tributanone oxime silane, cross-linking agent phenyltrimethoxysilane, mix well;

F. Add the catalyst stannous octoate and mix well, defoam; discharge and pack.

Claims (4)

1. a LED ketoxime removing type organosilicon sealant, is characterized in that: comprise the following raw material according to weight parts:

Hydroxyl-terminated injecting two methyl siloxane 80-100 part

Linking agent methyl three Diacetylmonoxime silane 15-25 part

Linking agent phenyltrimethoxysila,e 5-15 part

Stannous octoate 0.5-5 part

KH-5701.5-2.5 part

KH-7921.5-2.5 part

Dispersion agent 2-4 part

Pigments Chromium 5-9 part

Barium sulfate 30-38 part

Light calcium carbonate 30-36 part.

2. a kind of LED ketoxime removing type organosilicon sealant according to claim 1, is characterized in that: the viscosity of described hydroxyl-terminated injecting two methyl siloxane is 15000-20000mPas.

3. a kind of LED ketoxime removing type organosilicon sealant according to claim 1, is characterized in that: described dispersion agent is orthophosphoric acid salt.

4. the preparation method of a kind of LED ketoxime removing type organosilicon sealant according to claim 1, is characterized in that: comprise following processing step:

A, first hydroxyl-terminated injecting two methyl siloxane to be mixed in kneader with dispersion agent, Pigments Chromium, barium sulfate and light calcium carbonate;

B, temperature is risen to 135-145 DEG C, mediate in vacuum and stir 2-3h;

C, vacuum hydro-extraction 2-3h, cool the temperature to room temperature, and in three-roll grinder grinding evenly, discharging obtains base glue;

D, in homogenizer, add base glue, KH-570, KH-792;

E, vacuum hydro-extraction 2-3h, add linking agent methyl three Diacetylmonoxime silane, linking agent phenyltrimethoxysila,e, fully mix;

F, add the sub-tin of octoate catalyst and fully mix, deaeration; Discharging, packaging.