CN105112006A - Ketoxime-removal organosilicon sealant for LED (light-emitting diode) packaging and preparation method thereof - Google Patents
Ketoxime-removal organosilicon sealant for LED (light-emitting diode) packaging and preparation method thereof Download PDFInfo
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- CN105112006A CN105112006A CN201510568570.5A CN201510568570A CN105112006A CN 105112006 A CN105112006 A CN 105112006A CN 201510568570 A CN201510568570 A CN 201510568570A CN 105112006 A CN105112006 A CN 105112006A
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- CN
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- Prior art keywords
- parts
- led
- organosilicon sealant
- ketoxime
- linking agent
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Links
- 239000000565 sealant Substances 0.000 title claims abstract description 27
- 238000002360 preparation method Methods 0.000 title claims abstract description 14
- 238000004806 packaging method and process Methods 0.000 title claims abstract description 9
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 claims abstract description 26
- TZCXTZWJZNENPQ-UHFFFAOYSA-L barium sulfate Chemical compound [Ba+2].[O-]S([O-])(=O)=O TZCXTZWJZNENPQ-UHFFFAOYSA-L 0.000 claims abstract description 26
- -1 polydimethylsiloxane Polymers 0.000 claims abstract description 20
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 claims abstract description 15
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 claims abstract description 15
- 229910000077 silane Inorganic materials 0.000 claims abstract description 15
- 229910000019 calcium carbonate Inorganic materials 0.000 claims abstract description 13
- 239000000049 pigment Substances 0.000 claims abstract description 13
- KSBAEPSJVUENNK-UHFFFAOYSA-L tin(ii) 2-ethylhexanoate Chemical compound [Sn+2].CCCCC(CC)C([O-])=O.CCCCC(CC)C([O-])=O KSBAEPSJVUENNK-UHFFFAOYSA-L 0.000 claims abstract description 7
- 239000003795 chemical substances by application Substances 0.000 claims description 46
- 239000006185 dispersion Substances 0.000 claims description 18
- 239000000203 mixture Substances 0.000 claims description 15
- FSEUPUDHEBLWJY-HWKANZROSA-N diacetylmonoxime Chemical compound CC(=O)C(\C)=N\O FSEUPUDHEBLWJY-HWKANZROSA-N 0.000 claims description 13
- 239000003292 glue Substances 0.000 claims description 13
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 claims description 12
- 229910052804 chromium Inorganic materials 0.000 claims description 12
- 239000011651 chromium Substances 0.000 claims description 12
- 238000007599 discharging Methods 0.000 claims description 12
- 238000000605 extraction Methods 0.000 claims description 12
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical group OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims description 6
- 239000003054 catalyst Substances 0.000 claims description 6
- 238000000227 grinding Methods 0.000 claims description 6
- 125000005474 octanoate group Chemical group 0.000 claims description 6
- 239000002994 raw material Substances 0.000 claims description 6
- 238000003756 stirring Methods 0.000 claims description 6
- 238000004132 cross linking Methods 0.000 abstract description 2
- 239000003431 cross linking reagent Substances 0.000 abstract 5
- ZNOCGWVLWPVKAO-UHFFFAOYSA-N trimethoxy(phenyl)silane Chemical compound CO[Si](OC)(OC)C1=CC=CC=C1 ZNOCGWVLWPVKAO-UHFFFAOYSA-N 0.000 abstract 2
- WGLPBDUCMAPZCE-UHFFFAOYSA-N Trioxochromium Chemical compound O=[Cr](=O)=O WGLPBDUCMAPZCE-UHFFFAOYSA-N 0.000 abstract 1
- 239000004205 dimethyl polysiloxane Substances 0.000 abstract 1
- 239000002270 dispersing agent Substances 0.000 abstract 1
- 230000002349 favourable effect Effects 0.000 abstract 1
- 229920000435 poly(dimethylsiloxane) Polymers 0.000 abstract 1
- 239000000463 material Substances 0.000 description 5
- QTBSBXVTEAMEQO-UHFFFAOYSA-N acetic acid Substances CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 4
- 238000002156 mixing Methods 0.000 description 3
- 150000001412 amines Chemical class 0.000 description 2
- 125000000391 vinyl group Chemical group [H]C([*])=C([H])[H] 0.000 description 2
- 229920002554 vinyl polymer Polymers 0.000 description 2
- 230000001070 adhesive effect Effects 0.000 description 1
- 150000001408 amides Chemical class 0.000 description 1
- YHWCPXVTRSHPNY-UHFFFAOYSA-N butan-1-olate;titanium(4+) Chemical compound [Ti+4].CCCC[O-].CCCC[O-].CCCC[O-].CCCC[O-] YHWCPXVTRSHPNY-UHFFFAOYSA-N 0.000 description 1
- 230000003749 cleanliness Effects 0.000 description 1
- 238000009833 condensation Methods 0.000 description 1
- 230000005494 condensation Effects 0.000 description 1
- 230000018044 dehydration Effects 0.000 description 1
- 238000006297 dehydration reaction Methods 0.000 description 1
- KPUWHANPEXNPJT-UHFFFAOYSA-N disiloxane Chemical class [SiH3]O[SiH3] KPUWHANPEXNPJT-UHFFFAOYSA-N 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005538 encapsulation Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- NKSJNEHGWDZZQF-UHFFFAOYSA-N ethenyl(trimethoxy)silane Chemical compound CO[Si](OC)(OC)C=C NKSJNEHGWDZZQF-UHFFFAOYSA-N 0.000 description 1
- 239000000945 filler Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 125000004435 hydrogen atom Chemical group [H]* 0.000 description 1
- 238000000465 moulding Methods 0.000 description 1
- 229920001296 polysiloxane Polymers 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
- 229920002631 room-temperature vulcanizate silicone Polymers 0.000 description 1
- 238000007789 sealing Methods 0.000 description 1
- 229920002379 silicone rubber Polymers 0.000 description 1
- 239000004945 silicone rubber Substances 0.000 description 1
- 239000004590 silicone sealant Substances 0.000 description 1
- 150000003384 small molecules Chemical class 0.000 description 1
Landscapes
- Compositions Of Macromolecular Compounds (AREA)
- Sealing Material Composition (AREA)
Abstract
The invention relates to a ketoxime-removal organosilicon sealant for LED (light-emitting diode) packaging and a preparation method thereof, belonging to the technical field of organosilicon sealants. The organosilicon sealant comprises 80-100 parts of hydroxyl-terminated polydimethylsiloxane, 15-25 parts of crosslinking agent methyl tridiacetylmonoxime silane, 5-15 parts of crosslinking agent phenyltrimethoxy silane, 0.5-5 parts of stannous octoate, 1.5-2.5 parts of KH-570, 1.5-2.5 parts of KH-792, 2-4 parts of dispersing agent, 5-9 parts of pigment chromic oxide, 30-38 parts of barium sulfate and 30-36 parts of light calcium carbonate. By using the mixed crosslinking system composed of the ketoxime-removal crosslinking agent methyl tridiacetylmonoxime silane used as the main crosslinking agent and a small amount of dealcoholizing-type crosslinking agent phenyltrimethoxy silane, the single-component ketoxime-type organosilicon sealant has favorable comprehensive mechanical properties, and is very suitable for LED packaging.
Description
Technical field
The present invention relates to a kind of organosilicon sealant and preparation method thereof, more particularly, the present invention relates to a kind of LED ketoxime removing type organosilicon sealant and preparation method thereof, belong to organosilicon sealant technical field.
Background technology
One-component RTV silicone sealant refer to room temperature vulcanized silicone rubber and filler etc. is mixing after, add the component such as linking agent, catalyzer, and under thorough dehydration conditions with the form airtight package of single component, use and store, by absorbing a class organosilicon sealant product of the moisture-curable elastomer-forming in air.De-acetic acid type, ketoxime removing type, deacetone, de amide type, de-a few class such as amine type and dealcoholizing-type can be divided into by the small molecules kind removed during condensation.Ketoxime removing type organosilicon sealant due to adhesiveproperties good, the fast smell of curing speed is little, and corrodibility is less than acetic acid type and therefore amine type is widely used.
It is CN101935455A that State Intellectual Property Office discloses a publication number in 2011.1.5, name is called the invention of " a kind of LED organosilicon material and preparation method thereof ", this invention organosilicon material, it is characterized in that by component A be vinyl polysiloxane, B component is hydrogen containing siloxane, mix according to mass ratio 0.3:1 ~ 1:30, then add D component vinyl MQ resin, component E is one or more mixture and catalyzer component C in vinyltrimethoxy silane, tetrabutyl titanate, KH-560, be prepared from after mixing.The present invention needs another technical problem solved to be make preparation method's cleanliness without any pollution, and preparation method of the present invention, after proportionally each component being mixed, through room temperature in vacuo deaeration 5 ~ 30min, curing temperature is sulfidization molding at 20 ~ 150 DEG C.
The above-mentioned organosilicon material over-all properties for LED is poor.
Summary of the invention
The present invention is intended to the problem solving LED organosilicon material in prior art, and provide a kind of LED ketoxime removing type organosilicon sealant, sealing glue machine good combination property, is suitable for LED embedding very much.
In order to realize foregoing invention object, its concrete technical scheme is as follows:
A kind of 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.
The viscosity of hydroxyl-terminated injecting two methyl siloxane of the present invention is 15000-20000mPas.
Dispersion agent of the present invention is orthophosphoric acid salt.
A preparation method for LED ketoxime removing type organosilicon sealant, 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.
The Advantageous Effects that the present invention brings:
The invention solves for the poor problem of the organosilicon material over-all properties of LED.It is main linking agent that the present invention adopts with ketoxime removing type linking agent methyl three Diacetylmonoxime silane, add a small amount of dealcoholizing-type linking agent phenyltrimethoxysila,e simultaneously, composition mixing cross-linking system, prepare comprehensive mechanical property good single component ketoxime type organosilicon sealant, be applicable to very much the encapsulation of LED.
Embodiment
embodiment 1
A kind of LED ketoxime removing type organosilicon sealant, comprises the following raw material according to weight parts:
Hydroxyl-terminated injecting two methyl siloxane 80 parts
15 parts, linking agent methyl three Diacetylmonoxime silane
Linking agent phenyltrimethoxysila,e 5 parts
Stannous octoate 0.5 part
KH-5701.5 part
KH-7921.5 part
Dispersion agent 2 parts
Pigments Chromium 5 parts
30 parts, barium sulfate
Light calcium carbonate 30 parts.
embodiment 2
A kind of LED ketoxime removing type organosilicon sealant, comprises the following raw material according to weight parts:
Hydroxyl-terminated injecting two methyl siloxane 100 parts
25 parts, linking agent methyl three Diacetylmonoxime silane
Linking agent phenyltrimethoxysila,e 15 parts
Stannous octoate 5 parts
KH-5702.5 part
KH-7922.5 part
Dispersion agent 4 parts
Pigments Chromium 9 parts
38 parts, barium sulfate
Light calcium carbonate 36 parts.
embodiment 3
A kind of LED ketoxime removing type organosilicon sealant, comprises the following raw material according to weight parts:
Hydroxyl-terminated injecting two methyl siloxane 90 parts
20 parts, linking agent methyl three Diacetylmonoxime silane
Linking agent phenyltrimethoxysila,e 10 parts
Stannous octoate 2.75 parts
KH-5702 part
KH-7922 part
Dispersion agent 3 parts
Pigments Chromium 7 parts
34 parts, barium sulfate
Light calcium carbonate 33 parts.
embodiment 4
A kind of LED ketoxime removing type organosilicon sealant, comprises the following raw material according to weight parts:
Hydroxyl-terminated injecting two methyl siloxane 95 parts
21 parts, linking agent methyl three Diacetylmonoxime silane
Linking agent phenyltrimethoxysila,e 7 parts
Stannous octoate 1.5 parts
KH-5702.1 part
KH-7921.8 part
Dispersion agent 3.6 parts
Pigments Chromium 8 parts
35 parts, barium sulfate
Light calcium carbonate 35 parts.
embodiment 5
On the basis of embodiment 1-4:
Preferably, the viscosity of described hydroxyl-terminated injecting two methyl siloxane is 15000mPas.
Preferably, described dispersion agent is orthophosphoric acid salt.
embodiment 6
On the basis of embodiment 1-4:
Preferably, the viscosity of described hydroxyl-terminated injecting two methyl siloxane is 20000mPas.
Preferably, described dispersion agent is orthophosphoric acid salt.
embodiment 7
On the basis of embodiment 1-4:
Preferably, the viscosity of described hydroxyl-terminated injecting two methyl siloxane is 17500mPas.
Preferably, described dispersion agent is orthophosphoric acid salt.
embodiment 8
On the basis of embodiment 1-4:
Preferably, the viscosity of described hydroxyl-terminated injecting two methyl siloxane is 16000mPas.
Preferably, described dispersion agent is orthophosphoric acid salt.
embodiment 9
A preparation method for LED ketoxime removing type organosilicon sealant, comprises 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 DEG C, mediate in vacuum and stir 2h;
C, vacuum hydro-extraction 2h, 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 2h, 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.
embodiment 10
A preparation method for LED ketoxime removing type organosilicon sealant, comprises 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 145 DEG C, mediate in vacuum and stir 3h;
C, vacuum hydro-extraction 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 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.
embodiment 11
A preparation method for LED ketoxime removing type organosilicon sealant, comprises 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 140 DEG C, mediate in vacuum and stir 2.5h;
C, vacuum hydro-extraction 2.5h, 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 2.5h, 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.
embodiment 12
A preparation method for LED ketoxime removing type organosilicon sealant, comprises 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 138 DEG C, mediate in vacuum and stir 2.25h;
C, vacuum hydro-extraction 2.25h, 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 2.75h, 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.
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.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510568570.5A CN105112006A (en) | 2015-09-09 | 2015-09-09 | Ketoxime-removal organosilicon sealant for LED (light-emitting diode) packaging and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510568570.5A CN105112006A (en) | 2015-09-09 | 2015-09-09 | Ketoxime-removal organosilicon sealant for LED (light-emitting diode) packaging and preparation method thereof |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN105112006A true CN105112006A (en) | 2015-12-02 |
Family
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201510568570.5A Pending CN105112006A (en) | 2015-09-09 | 2015-09-09 | Ketoxime-removal organosilicon sealant for LED (light-emitting diode) packaging and preparation method thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN105112006A (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105925200A (en) * | 2016-05-06 | 2016-09-07 | 烟台图文马克化工科技有限公司 | Silicone sealant for automotive chassis |
| CN106753197A (en) * | 2017-02-14 | 2017-05-31 | 中卫市创科知识产权投资有限公司 | A kind of organic silicone adhesive agent producing process |
| CN112080246A (en) * | 2020-08-31 | 2020-12-15 | 仲恺农业工程学院 | A kind of silicone potting glue and preparation method thereof |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2006106362A1 (en) * | 2005-04-06 | 2006-10-12 | Dow Corning Corporation | Organosiloxane compositions |
| CN104388040A (en) * | 2014-10-23 | 2015-03-04 | 中国航空工业集团公司北京航空材料研究院 | Single-component flame-retardant ketoxime-removed/dealcoholized room temperature vulcanized organosilicon sealant and preparation method thereof |
-
2015
- 2015-09-09 CN CN201510568570.5A patent/CN105112006A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2006106362A1 (en) * | 2005-04-06 | 2006-10-12 | Dow Corning Corporation | Organosiloxane compositions |
| CN104388040A (en) * | 2014-10-23 | 2015-03-04 | 中国航空工业集团公司北京航空材料研究院 | Single-component flame-retardant ketoxime-removed/dealcoholized room temperature vulcanized organosilicon sealant and preparation method thereof |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105925200A (en) * | 2016-05-06 | 2016-09-07 | 烟台图文马克化工科技有限公司 | Silicone sealant for automotive chassis |
| CN106753197A (en) * | 2017-02-14 | 2017-05-31 | 中卫市创科知识产权投资有限公司 | A kind of organic silicone adhesive agent producing process |
| CN112080246A (en) * | 2020-08-31 | 2020-12-15 | 仲恺农业工程学院 | A kind of silicone potting glue and preparation method thereof |
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Application publication date: 20151202 |