CN104449546B - Environment-friendly type LED light fixture joint sealant and preparation method thereof - Google Patents

Environment-friendly type LED light fixture joint sealant and preparation method thereof Download PDF

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CN104449546B
CN104449546B CN201410664829.1A CN201410664829A CN104449546B CN 104449546 B CN104449546 B CN 104449546B CN 201410664829 A CN201410664829 A CN 201410664829A CN 104449546 B CN104449546 B CN 104449546B
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deaeration
preparation
catalyst
led light
light fixture
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CN104449546A (en
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翁祝强
刘金明
张彬
黄永军
陈超
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Zhaoshun Technology (Guangdong) Co., Ltd
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Dongguan Million Shun's Organosilicon Science And Technology Co Ltd
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Abstract

A kind of environment-friendly type LED light fixture joint sealant and preparation method thereof.The present invention is base glue with (α, ω) dialkyl polydimethylsiloxane, adds filler, deaeration, adds crosslinking agent, deaeration after being down to room temperature;It is subsequently adding catalyst, deaeration, prepare environment-friendly type LED light fixture joint sealant.Used catalyst of the present invention is organosilicon titanium complex, and its structural formula is: Ti [O (C3H6O)m(C2H4O)nH]a[(OSi(CH3)2)hOSi(CH3)3](4‑a), wherein, 3 >=a >=0 and be integer, 1000 > m, n, h > 50.The fluid sealant preparing has the features such as corrosion-free, yellowing resistance good, caking property is excellent.

Description

Environment-friendly type LED light fixture joint sealant and preparation method thereof
Technical field
The invention belongs to fluid sealant technical field, be specifically related to a kind of corrosion-free, yellowing resistance good, caking property Excellent fluid sealant, for the adhering and sealing of LED lamp lampshade and pedestal.
Background technology
Single-component dealcoholization-type room temperature vulcanized silicone rubber for electron trade is most for de-ethanol in the market Type, minority is piptonychia alcohol type.De-ethanol-type used catalyst is for such as diethylin MTES etc. High activity aminated compounds or organic tin catalyst.In aminated compounds amino in use aoxidize flavescence and Corrosion can be produced;Organic tin catalyst (dibutyl tin laurate, stannous octoate etc.) itself is toxic, Can release organic acid in using solidification process, organic acid can occur xanthochromia and produce corrosion to base material.
From 2009, in EC regulations REACH clearly propose prohibit the use of dibutyl tin and dioctyl tin and Three replacement tin compounds.Piptonychia alcohol type used catalyst in the market is most for double (ethyl acetoacetate) This is several alone for metatitanic acid diisopropyl ester, two (levulinic ketone group) metatitanic acid diisopropyl ester, organic tin catalyst Or collocation uses.Owing to ethyl acetoacetate and acetylacetone,2,4-pentanedione at high temperature easily turn yellow, at the double (acetyl of synthesis Ethyl acetate) metatitanic acid diisopropyl ester and the catalyst obtaining during two (levulinic ketone group) metatitanic acid diisopropyl ester many Number is bronzing and yellow liquid, and ethyl acetoacetate or acetylacetone,2,4-pentanedione are released in solidification when being used as RTV catalyst Thus cause fluid sealant surface to turn to be yellow;During in addition, they are used as catalyst, the reason that due to this body structure, Still need to add other amine silane couplers increasing its caking property to material, thus cause its xanthochromia and Corrosion problems increases the weight of.
And it is used alone titanate esters as catalyst and without amine silane coupler, organic tin catalyst, Not groups such as amino-contained, ethyl acetoacetate, acetylacetone,2,4-pentanedione in system, this type of fluid sealant is not reported.
Content of the invention
For the technical deficiency of existing single-component dealcoholization-type room temperature vulcanized silicone rubber, it is an object of the invention to provide A kind of fluid sealant being mainly used in LED lamp lampshade and the adhering and sealing of pedestal.The fluid sealant of the present invention is without corruption Erosion, color inhibition, caking property are excellent.
For reaching above-mentioned purpose, the present invention adopts the following technical scheme that
A kind of environment-friendly type LED light fixture joint sealant, material component is based on following mass parts:
As optimal technical scheme, environment-friendly type LED light fixture joint sealant of the present invention, described (α, The dynamic viscosity of ω)-dialkyl polydimethylsiloxane is 500~500000cps, for example, 550cps, 1000 cps、5000cps、8000cps、15000cps、50000cps、80000cps、200000cps、450000 Cps etc..The fluid sealant that (α, ω)-dialkyl polydimethylsiloxane in above-mentioned range of viscosities prepares has Preferable toughness, extrudability, hardness.
As optimal technical scheme, environment-friendly type LED light fixture joint sealant of the present invention, described filler For any one in calcium carbonate, titanium dioxide, white carbon, zinc oxide, silicon powder or two or more Combination.
As optimal technical scheme, environment-friendly type LED light fixture joint sealant of the present invention, described crosslinking Agent is methyl silicate, MTMS, vinyltrimethoxy silane, dodecyl trimethoxy In base silane, phenyltrimethoxysila,e, allyltrimethoxysilanis any one or two or more Combination.
As optimal technical scheme, environment-friendly type LED light fixture joint sealant of the present invention, described catalysis Agent is titanate catalyst, its structural formula such as following formula (1):
Ti[O(C3H6O)m(C2H4O)nH]a[(OSi(CH3)2)hOSi(CH3)3](4-a) (1)
Wherein, 3 >=a >=0 and be integer, 1000 > m, n, h > 50.
Titaniferous condensed type catalyst above-mentioned in the present invention can use following preparation method, comprises the steps:
1) pre-treatment: be passed through inert gas in tetraisopropyl titanate;
2) prepare mixture: PPG is mixed with hydroxy silicon oil, prepares mixture;
3) react: described mixture is added drop-wise to described tetraisopropyl titanate reacts;
4) post-process: reacted lower-molecular substance is removed, obtains titaniferous condensed type catalyst.
The catalyst of the present invention is prepared from by tetraisopropyl titanate, PPG and hydroxy silicon oil, wherein The Si-O key containing in hydroxy silicon oil has effect and the increase catalyst of Ti-key in stable tetraisopropyl titanate Effect with siloxanes compatibility;The introducing of PPG so that described catalyst water absorbing capacity strengthens, So that the ability to cure of described catalyst significantly improves.
Described lower-molecular substance is isopropanol.
Step 1) described inert gas be passed through the time for more than 30min.Described inert gas be nitrogen and / or helium.
The mass ratio of described tetraisopropyl titanate and described mixture is 1:2-10, as 1:3,1:4,1:5,1:6, 1:7,1:8 or 1:9 etc..
Step 3) described reaction is by step 2) described mixture is added drop-wise in described tetraisopropyl titanate, choosing Mode with dropping so that react more uniform, stable;The reaction time of described reaction is 0.5-6h, as 1h, 2h, 3h, 4h, 4.5h, 5h or 5.5h etc.;The temperature of described reaction be not higher than 80 DEG C, as 10 DEG C, 20 DEG C, 25 DEG C, 30 DEG C, 40 DEG C, 45 DEG C, 50 DEG C, 60 DEG C, 70 DEG C or 75 DEG C etc., preferably 60 DEG C.
Step 2) described PPG is arbitrary with the mol ratio of hydroxy silicon oil, preferably 1:1-3, as 1:1.2,1:1.5,1:1.8,1:2,1:2.3,1:2.5,1:2.8 or 1:2.9 etc..Described reaction system will be to gather Based on siloxanes, the catalyst and the polysiloxanes that so prepare can similar compatibility, improve at polysiloxanes Solubility.
The weight average molecular weight of described PPG is 300-800, as the 350th, the 400th, the 450th, the 500th, the 600th, 650th, 700 or 750 etc., the weight average molecular weight of described hydroxy silicon oil is 200-600, as the 250th, the 300th, the 350th, 380th, the 400th, the 450th, 500 or 550 etc..Consider for reactivity and catalysis activity, select as mentioned above The PPG of molecular weight and hydroxy silicon oil: if the molecular weight of PPG and hydroxy silicon oil is smaller, The catalyst of preparation is unstable;Molecular weight is bigger, and the catalyst activity preparing is bad, catalysis Speed is too slow.
Preferably, described PPG weight average molecular weight is the polyether Glycols of 500, as HO(C2H4O)8(C3H6O)8H;Described hydroxy silicon oil weight average molecular weight is 500, such as HO ((CH3)2SiO)7H。
Step 4) described removing lower-molecular substance device be chemical industry common equipment.Described removal temperature is the highest not More than 80 DEG C, such as 10 DEG C, 20 DEG C, 25 DEG C, 30 DEG C, 40 DEG C, 45 DEG C, 50 DEG C, 60 DEG C, 70 DEG C or 75 DEG C. Described removing lower-molecular substance proceeds to flow out without low molecule, and the time does not limits.
Titaniferous condensed type catalyst above-mentioned in the present invention also can use other any suitable method systems Standby.
An object of the present invention also resides in a kind of environment-friendly type LED light fixture joint sealant of the present invention Preparation method, comprises the following steps:
(1) in (α, ω)-dialkyl polydimethylsiloxane, filler being added power mixer according to quantity, The lower deaeration of heating;
(2) crosslinking agent, deaeration are added after being down to room temperature;
(3) it is subsequently adding catalyst, deaeration, obtain described fluid sealant.
As optimal technical scheme, the preparation method of the present invention, the temperature of the described heating of step (1) is 120 DEG C ~200 DEG C.
Preferably, described deaeration is-0.15-0.03MPa in vacuum, carries out under preferably-0.08MPa stirring 3~10 hours.
As optimal technical scheme, the preparation method of the present invention, the described deaeration of step (2) in vacuum is Carry out 10~60 minutes under-0.15-0.03MPa, preferably-0.08MPa stirring.
As optimal technical scheme, the preparation method of the present invention, the described deaeration of step (3) in vacuum is Carry out 10~120 minutes under-0.15-0.03MPa, preferably-0.08MPa stirring.
As optimal technical scheme, the preparation method of the present invention, comprise the steps:
(1) power is added to mix according to quantity (α, ω)-dialkyl polydimethylsiloxane, plasticizer, filler In conjunction machine, under the conditions of temperature 120 DEG C~200 DEG C, vacuum-0.08MPa, stir deaeration 3~10 hours;
(2) add crosslinking agent after being down to room temperature, under vacuum-0.08MPa, stir deaeration 30 minutes;
(3) it is subsequently adding catalyst, stir deaeration 30~60 minutes under vacuum;Discharging, packaging.
Used catalyst of the present invention has without corruption for self-control organosilicon titanium complex, the fluid sealant that the present invention prepares The features such as erosion, yellowing resistance is good, caking property is excellent.
Detailed description of the invention
For the present invention is better described, it is simple to understand technical scheme, the typical case of the present invention but non-limit The embodiment of property processed is as follows:
Embodiment 1:
A kind of environment-friendly type LED light fixture joint sealant, material component is based on following mass parts:
And adopt and prepare with the following method:
(1) in (α, ω)-dialkyl polydimethylsiloxane, filler being added power mixer according to quantity, Deaeration 3~10 hours is stirred under the conditions of temperature 200 DEG C, vacuum-0.08MPa;
(2) add crosslinking agent after being down to room temperature, under vacuum-0.08MPa, stir deaeration 30 minutes;
(3) it is subsequently adding catalyst, stir deaeration 60 minutes under vacuum and get final product.
Embodiment 2
A kind of environment-friendly type LED light fixture joint sealant, material component is based on following mass parts:
And adopt and prepare with the following method:
(1) in (α, ω)-dialkyl polydimethylsiloxane, filler being added power mixer according to quantity, Deaeration 3 hours is stirred under the conditions of temperature 120 DEG C, vacuum-0.03MPa;
(2) add crosslinking agent after being down to room temperature, under vacuum-0.12MPa, stir deaeration 10 minutes;
(3) it is subsequently adding catalyst, stir deaeration 10 minutes under vacuum and get final product.
Embodiment 3
A kind of environment-friendly type LED light fixture joint sealant, material component is based on following mass parts:
And adopt and prepare with the following method:
(1) in (α, ω)-dialkyl polydimethylsiloxane, filler being added power mixer according to quantity, Deaeration 10 hours is stirred under the conditions of temperature 160 DEG C, vacuum-0.14MPa;
(2) add crosslinking agent after being down to room temperature, under vacuum-0.03MPa, stir deaeration 30 minutes;
(3) it is subsequently adding catalyst, stir deaeration 60 minutes under vacuum and get final product.
The fluid sealant that embodiment 1-3 prepares is carried out performance test, and testing result is shown in Table 1.
Table 1
From the results shown in Table 1, the environment-friendly type LED light fixture joint sealant caking property that prepared by the present invention Good, anti-yellowing property is excellent, it is adaptable to the adhering and sealing of LED lamp.
Applicant states, the present invention illustrates the method detailed of the present invention by above-described embodiment, but the present invention It is not limited to above-mentioned method detailed, i.e. do not mean that the present invention has to rely on above-mentioned method detailed and could implement. Person of ordinary skill in the field is it will be clearly understood that any improvement in the present invention, each former to product of the present invention The interpolation of the equivalence replacement of material and auxiliary element, concrete way choice etc., all fall within the protection model of the present invention Within the scope of enclosing and disclosing.

Claims (5)

1. an environment-friendly type LED light fixture joint sealant, material component is based on following mass parts:
The dynamic viscosity of described (α, ω)-dialkyl polydimethylsiloxane is 500~8000cps;
Described filler be titanium dioxide, white carbon, zinc oxide, any one or two kinds in silicon powder with On combination;
Described crosslinking agent be methyl silicate, MTMS, vinyltrimethoxy silane, ten Any one in dialkyl group trimethoxy silane, phenyltrimethoxysila,e, allyltrimethoxysilanis Or two or more combinations;
Described catalyst is titanate catalyst, its structure such as formula (1):
Ti[O(C3H6O)m(C2H4O)nH]a[(OSi(CH3)2)hOSi(CH3)3](4-a) (1)
Wherein, 3 >=a >=0 and be integer, 1000 > m, n, h > 50.
2. a preparation method for the environment-friendly type LED light fixture joint sealant described in claim 1, including Following steps:
(1) in (α, ω)-dialkyl polydimethylsiloxane, filler being added power mixer according to quantity, The lower deaeration of heating;
(2) crosslinking agent, deaeration are added after being down to room temperature;
(3) it is subsequently adding catalyst, deaeration, obtain described fluid sealant.
3. preparation method according to claim 2, it is characterised in that the described heating of step (1) Temperature is 120 DEG C~200 DEG C.
4. preparation method according to claim 2, it is characterised in that the described deaeration of step (2) exists Vacuum is stirring 10~60 minutes under the conditions of-0.15-0.03MPa.
5. preparation method according to claim 2, it is characterised in that comprise the steps:
(1) in (α, ω)-dialkyl polydimethylsiloxane, filler being added power mixer according to quantity, Deaeration 3~10 hours is stirred under the conditions of temperature 120 DEG C~200 DEG C, vacuum-0.08MPa;
(2) add crosslinking agent after being down to room temperature, under vacuum-0.08MPa, stir deaeration 30 minutes;
(3) it is subsequently adding catalyst, stir deaeration 30~60 minutes under vacuum;Discharging, packaging.
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CN105860861A (en) * 2016-05-06 2016-08-17 烟台图文马克化工科技有限公司 Silicone sealant for hanging wallboard
CN113185546B (en) * 2021-04-28 2022-07-29 广州市白云化工实业有限公司 High-activity catalyst for dealcoholized silicone sealant and preparation method and application thereof

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Publication number Priority date Publication date Assignee Title
CN102146208A (en) * 2011-01-26 2011-08-10 广州市高士实业有限公司 Method for preparing transparent dealcoholized single-component room temperature vulcanized silicone rubber
CN102757647A (en) * 2012-07-11 2012-10-31 东莞兆舜有机硅新材料科技有限公司 Single-component catalytic dealcoholized room temperature vulcanized (RTV) silicone rubber and preparation method thereof

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CN103951980B (en) * 2013-09-18 2017-02-08 烟台德邦科技有限公司 Wet-heat dual curing silicone composition

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102146208A (en) * 2011-01-26 2011-08-10 广州市高士实业有限公司 Method for preparing transparent dealcoholized single-component room temperature vulcanized silicone rubber
CN102757647A (en) * 2012-07-11 2012-10-31 东莞兆舜有机硅新材料科技有限公司 Single-component catalytic dealcoholized room temperature vulcanized (RTV) silicone rubber and preparation method thereof

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Address after: Two street 523233 Guangdong province Dongguan City Chudo Zhen Dong Bo Cun Da Xin Wei Lu Daxin Road No. 1

Applicant after: Dongguan million Shun's organosilicon Science and Technology Co., Ltd.

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Free format text: CORRECT: APPLICANT; FROM: DONGGUAN ZHAOSHUN ORGANOSILICON NEW MATERIAL TECHNOLOGY CO., LTD . TO: DONGGUAN MEGASUN SILICONE TECHNOLOGY CO., LTD.

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Address after: Two street 523233 Guangdong province Dongguan City Chudo Zhen Dong Bo Cun Da Xin Wei Lu Daxin Road No. 1

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Address before: Two street 523233 Guangdong province Dongguan City Chudo Zhen Dong Bo Cun Da Xin Wei Lu Daxin Road No. 1

Patentee before: Dongguan million Shun's organosilicon Science and Technology Co., Ltd.