CN109735297A - A kind of organosilicon sealant and preparation method thereof that fugitive constituent is controlled - Google Patents
A kind of organosilicon sealant and preparation method thereof that fugitive constituent is controlled Download PDFInfo
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- CN109735297A CN109735297A CN201811578876.9A CN201811578876A CN109735297A CN 109735297 A CN109735297 A CN 109735297A CN 201811578876 A CN201811578876 A CN 201811578876A CN 109735297 A CN109735297 A CN 109735297A
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Abstract
The invention belongs to polymeric material fields, are related to a kind of organosilicon sealant and preparation method thereof that fugitive constituent is controlled.Component is as follows by weight: α, 100 parts of alpha, omega-dihydroxy polydimethyl siloxane, 5~25 parts of dimethicone, 100~160 parts of calcium carbonate, 5~25 parts of carbon black, 1~10 part of fumed silica, 5~30 parts of crosslinking agent, 0.1~2 part of coupling agent, 5~10 parts of catalyst.α of the present invention, low molecule content in alpha, omega-dihydroxy polydimethyl siloxane and dimethicone is 100~300ppm, and the controlled organosilicon sealant of fugitive constituent is prepared in conjunction with precise process, its is environmentally friendly, storage is stable, ageing-resistant performance and excellent to the adhesive property of a variety of substrates, can be used for building, the multiple fields such as automobile, electronic apparatus and medical instrument.
Description
Technical field
The invention belongs to polymeric material field more particularly to a kind of organosilicon sealant that fugitive constituent is controlled and its preparations
Method.
Background technique
Organosilicon sealant is due to easy to use, moderate cost and excellent comprehensive performance, in building, automobile, electronics electricity
The multiple fields such as device, medical machinery are used widely.Low molecular weight volatile part in organosilicon sealant can gradually be escaped from glue
Out, it is attached in other materials, generates material transmitance, many bad phenomenons such as photoelectric properties, coating surface change, lead
Material lifetime is caused to shorten, using adverse consequences such as failure, security risks.In addition, high-volatile is to organosilicon sealant itself
Ageing-resistant performance, adhesive property etc. have adverse effect.In actual use, in addition to requiring basic physical and chemical performance and stabilization
Property outside, every field to the control of the content of fugitive constituent be increasingly stringenter with urgently.Therefore, safe and reliable stable, environmental protection, scale
The controlled organosilicon sealant of fugitive constituent is prepared as inexorable trend.
Summary of the invention
The purpose of the present invention is being directed to deficiency and actual demand of the existing organosilicon sealant about fugitive constituent control technology,
And provide a kind of organosilicon sealant and preparation method thereof that fugitive constituent is controlled.The organosilicon sealant preparation method safely may be used
It leans on, stability is good, is suitble to assembly line large-scale production.
The technical solution of the present invention is as follows: a kind of organosilicon sealant that fugitive constituent is controlled, it is characterised in that its material component
And the parts by weight of each component are as follows:
Low molecular weight polycaprolactone content of siloxane is 100 in wherein α, alpha, omega-dihydroxy polydimethyl siloxane and dimethicone
~300ppm.
It is preferred that above-mentioned α, viscosity of the alpha, omega-dihydroxy polydimethyl siloxane at 25 DEG C is 1500~80000mPas.
It is preferred that viscosity of the above-mentioned dimethicone at 25 DEG C is 350~1000mPas.
It is preferred that above-mentioned calcium carbonate is one or both of nm-class active calcium carbonate or powdered whiting.It is preferred that above-mentioned
Fumed silica is hydrophobic type, and specific surface area is 150~380m2/g。
It is preferred that above-mentioned crosslinking agent is methyl orthosilicate, ethyl orthosilicate, methyltrimethoxysilane, methyl triethoxy
Silane, vinyltrimethoxysilane, vinyltriethoxysilane, phenyltrimethoxysila,e or phenyl triethoxysilane
At least one of.It is preferred that above-mentioned coupling agent is at least one of KH470, KH550, KH560, KH570 or KH792.
It is preferred that above-mentioned catalyst is isopropyl titanate, two (ethyl acetoacetate) titanium diisopropyl esters, bis- (acetylacetone,2,4-pentanediones)
One of metatitanic acid diisopropyl ester or bis- (acetylacetone,2,4-pentanedione) metatitanic acid diisobutyl esters.
The present invention also provides the methods of above-mentioned organosilicon sealant, the specific steps of which are as follows:
(1) first stearic acid modified calcium carbonate, carbon black and fumed silica are dried；
(2) then by α, alpha, omega-dihydroxy polydimethyl siloxane, dimethicone, calcium carbonate, carbon black and gas phase titanium dioxide
Silicon is added in (preferably planet) blender, and 2~4h is stirred and be dehydrated at 100~120 DEG C, -0.09~-0.1MPa, is mixed
Close uniform sizing；
(3) by the cooling addition reaction kettle of sizing, crosslinking agent is added, and stir under recirculated cooling water and vacuum environment
Mix mixing 10~15 minutes；
(4) coupling agent and catalyst is added under nitrogen atmosphere again, keeps recirculated cooling water, stirs 20~40 points after premix
Clock；
(5) it reduces mixing speed and stirs and persistently vacuumize 1~2h stopping, discharging, wrap after being filled with nitrogen to normal pressure in kettle
Dress, obtains product.
Mixing speed in preferred steps (3) and (4) is 600~800 revs/min；Mixing speed in step (5) is
50~100 revs/min.
Low molecular weight polycaprolactone content of siloxane α of the present invention, alpha, omega-dihydroxy polydimethyl siloxane and dimethicone are excellent
Following methods are selected to be made, specific steps are as follows:
(1) silicon rubber is placed in vacuum drying oven drying；
(2) silicon rubber obtained step (1) is added in removing means, 120~180 DEG C, 100~200Pa vacuum degree,
It is handled under 5~10L/h silicon rubber flow velocity；
(3) silicon rubber for obtaining step (2) is added in removing means, in 150~250 DEG C, 10~150Pa vacuum degree, 1
It is handled under~5L/h silicon rubber flow velocity, obtains the silicon rubber of removing low molecular weight polycaprolactone siloxanes.
The temperature of baking oven is 100~150 DEG C in preferred steps (1), and drying time is 24~72h.
Removing means in above-mentioned steps (2) and step (3) is thin film evaporator, vacuum distillation device or short-distance distiller
One of, market is on sale.
Number of processes is 1~5 time in above-mentioned steps (2), and number of processes is 1~6 time in step (3).
Treatment temperature of the treatment temperature ratio in step (2) in above-mentioned steps (3) is 30~70 DEG C high.
The utility model has the advantages that
Controlled organosilicon sealant of a kind of fugitive constituent according to the present invention and preparation method thereof has the following characteristics that
(1) the low molecule content in starting material α, alpha, omega-dihydroxy polydimethyl siloxane and dimethicone is 100
The fugitive constituent in finished product organosilicon sealant can be effectively controlled in~300ppm.
(2) by reasonably formula and fining technique, can safety and stability prepare organosilicon sealant, while being suitble to advise
Modelling production.
Specific embodiment
Example 1
By the α that viscosity is 20000mPas, low molecular weight polycaprolactone content of siloxane is 18000ppm at 25 DEG C, alpha, omega-dihydroxy is poly-
Dimethyl siloxane is placed in vacuum drying oven, handled at 100 DEG C for 24 hours afterwards be added thin film evaporator in, 120 DEG C, 100Pa it is true
It handles 5 times, is added in vacuum distillation device again, in 150 DEG C, 150Pa vacuum degree, 5L/h silicon rubber stream under reciprocal of duty cycle, 10L/h flow velocity
Speed lower processing 6 times, obtain the α, ω-two that viscosity is 20000mPas at 25 DEG C that low molecular weight polycaprolactone content of siloxane is 100ppm
Hydroxyl dimethyl silicone polymer.
The dimethicone that viscosity is 500, low molecular weight polycaprolactone content of siloxane is 22000ppm at 25 DEG C is placed in vacuum to dry
In case, it is added in vacuum distillation device after 48h is handled at 120 DEG C, handles 1 under 150 DEG C, 180Pa vacuum degree, 8L/h flow velocity
It is secondary, it is added in short-distance distiller again, is handled 1 time under 200 DEG C, 100Pa vacuum degree, 4L/h silicon rubber flow velocity, obtain low point
The dimethicone that viscosity is 500mPas at sub- polysiloxane level is 25 DEG C of 160ppm.
By 20000mPas, the α that low molecule content is 100ppm, 100 parts of alpha, omega-dihydroxy polydimethyl siloxane with
500mPas, 10 parts of dimethicone that low molecule content is 260ppm, 15 parts of 100 parts of calcium carbonate, carbon black, gas after drying
Aerosil (specific surface area 150m2/ g) 10 parts be added in planetary mixer, stir and be dehydrated at 110 DEG C, -0.1MPa
2h obtains uniformly mixed sizing, and sizing is added 8 parts of methyltrimethoxysilane after being cooled to 30 DEG C, cold recycling
But water is to mix 12 minutes under 600 revs/min with vacuum environment, mixing speed, is added 0.5 part under 30 DEG C of Yu Wendu and nitrogen atmosphere
KH550 and 5 part of bis- (acetylacetone,2,4-pentanedione) metatitanic acid diisopropyl ester keeps recirculated cooling water, premixes and low whipping speed is 600 revs/min
After continuing stirring 30 minutes, reducing mixing speed is that 1.5h stopping persistently being stirred and vacuumized under 80 revs/min, is filled with nitrogen in kettle
It discharges after to normal pressure, packs, obtain product.
Example 2
By viscosity 5000mPas, the α that low molecular weight polycaprolactone content of siloxane is 16000ppm, alpha, omega-dihydroxy poly- two at 25 DEG C
Methylsiloxane is placed in vacuum drying oven, and is added in thin film evaporator after 48h is handled at 150 DEG C, in 180 DEG C, 200Pa vacuum
It handles 1 time, is added in vacuum distillation device again, under 250 DEG C, 10Pa vacuum degree, 2L/h silicon rubber flow velocity under degree, 8L/h flow velocity
Processing 1 time, obtains the α that viscosity is 5000mPas at 25 DEG C that low molecular weight polycaprolactone content of siloxane is 300ppm, and alpha, omega-dihydroxy is poly-
Dimethyl siloxane.
The dimethicone that viscosity is 1000mPas, low molecular weight polycaprolactone content of siloxane is 22000ppm at 25 DEG C is placed in
In vacuum drying oven, it is added in vacuum distillation device after 48h is handled at 130 DEG C, under 140 DEG C, 150Pa vacuum degree, 8L/h flow velocity
Processing 3 times is added in short-distance distiller again, handles 2 times, obtain under 190 DEG C, 100Pa vacuum degree, 3L/h silicon rubber flow velocity
The dimethicone that viscosity is 1000mPas at low molecular weight polycaprolactone content of siloxane is 25 DEG C of 130ppm.
By the α that viscosity is 5000mPas, low molecule content is 300ppm, 100 parts of alpha, omega-dihydroxy polydimethyl siloxane
With 8 parts of dimethicone that viscosity is 1000mPas, low molecule content is 150ppm, 140 parts of calcium carbonate, carbon black after drying
8 parts of 20 parts, fumed silica (specific surface area 380m2/ g) it is added in planetary mixer, it is stirred at 100 DEG C, -0.09MPa
It mixes and is dehydrated 4h and obtain uniformly mixed sizing, vinyltrimethoxysilane 12 is added after being cooled to 30 DEG C in sizing
Part, it is mixed 10 minutes under being 800 revs/min with vacuum environment, mixing speed in recirculated cooling water, 30 DEG C of Yu Wendu and nitrogen atmosphere
0.8 part KH792 and 7 part two (ethyl acetoacetate) titanium diisopropyl ester of lower addition keeps recirculated cooling water, premixes and in stirring speed
Degree is after continuing stirring under 800 revs/min 25 minutes, and reducing mixing speed is that 1h stopping persistently being stirred and vacuumized under 50 revs/min,
It discharges after being filled with nitrogen to normal pressure in kettle, packs, obtain product.
Example 3
By 50000mPas, the α that low molecular weight polycaprolactone content of siloxane is 20000ppm, alpha, omega-dihydroxy polydimethyl at 25 DEG C
Siloxanes is placed in vacuum drying oven, at 140 DEG C handle 64h after be added thin film evaporator in, 160 DEG C, 150Pa vacuum degree,
It handles 2 times, is added in vacuum distillation device again, under 200 DEG C, 50Pa vacuum degree, 2L/h silicon rubber flow velocity under 6L/h flow velocity
Reason 2 times obtains the α of 50000mPas at 25 DEG C that low molecular weight polycaprolactone content of siloxane is 200ppm, alpha, omega-dihydroxy polydimethyl
Siloxanes.
The dimethicone that viscosity is 350mPas, low molecular weight polycaprolactone content of siloxane is 20000ppm at 25 DEG C is placed in
In vacuum drying oven, it is added in vacuum distillation device after 48h is handled at 120 DEG C, under 150 DEG C, 180Pa vacuum degree, 8L/h flow velocity
Processing 3 times is added in short-distance distiller again, handles 5 times, obtain under 200 DEG C, 100Pa vacuum degree, 4L/h silicon rubber flow velocity
The dimethicone that viscosity is 350mPas at low molecular weight polycaprolactone content of siloxane is 25 DEG C of 100ppm.
By the α that viscosity is 50000mPas, low molecule content is 200ppm, alpha, omega-dihydroxy polydimethyl siloxane 100
Part is with 20 parts of dimethicone that viscosity is 350mPas, low molecule content is 100ppm, 160 parts of calcium carbonate, charcoal after drying
Black 5 parts, fumed silica (specific surface area 200m2/ g) 3 parts be added in planetary mixer, stirred at 120 DEG C, -0.1MPa
It mixes and is dehydrated 4h and obtain uniformly mixed sizing, methyltrimethoxysilane 25 is added after being cooled to 30 DEG C in sizing
Part, it is mixed 15 minutes under being 700 revs/min with vacuum environment, mixing speed in recirculated cooling water, 30 DEG C of Yu Wendu and nitrogen atmosphere
2 parts KH570 and 10 part bis- (acetylacetone,2,4-pentanedione) metatitanic acid diisobutyl ester of lower addition keeps recirculated cooling water, premixes simultaneously low whipping speed
It is after continuing stirring under 800 revs/min 35 minutes, reducing mixing speed is that 2h stopping persistently being stirred and vacuumized under 100 revs/min,
It discharges after being filled with nitrogen to normal pressure in kettle, packs, obtain product.
Comparative example 1
By 20000mPas, the α that low molecule content is 14000ppm, 100 parts of alpha, omega-dihydroxy polydimethyl siloxane with
500mPas, low molecule content are 10 parts of dimethicone of 16000ppm, 15 parts of 100 parts of calcium carbonate, carbon black after drying,
In 10 parts of addition planetary mixers of fumed silica, stirred at 110 DEG C, -0.1MPa and be dehydrated 4h obtain it is uniformly mixed
Sizing, sizing is added 8 parts of methyltrimethoxysilane after being cooled to 30 DEG C, under recirculated cooling water and vacuum environment
0.5 part KH550 and 5 part bis- (acetylacetone,2,4-pentanedione) metatitanic acid diisopropyl ester is added under mixing 12 minutes, 30 DEG C of Yu Wendu and nitrogen atmosphere,
Recirculated cooling water is kept, premixes and persistently stirs and vacuumize after continuing stirring 30 minutes 1.5h stopping, being filled with nitrogen extremely in kettle
It discharges after normal pressure, packs, obtain product.
Comparative example 2
By 5000mPas, the α that low molecule content is 18000ppm, 100 parts of alpha, omega-dihydroxy polydimethyl siloxane with
1000mPas, low molecule content are 8 parts of dimethicone of 15000ppm, 20 parts of 140 parts of calcium carbonate, carbon black after drying,
In 8 parts of addition planetary mixers of fumed silica, stirred at 100 DEG C, -0.09MPa and be dehydrated 4h obtain it is uniformly mixed
Sizing, sizing is added 12 parts of vinyltrimethoxysilane after being cooled to 30 DEG C, in recirculated cooling water and vacuum ring
It is mixed 10 minutes under border, 0.8 part KH792 and 7 part two (ethyl acetoacetate) titanium two is added under 30 DEG C of Yu Wendu and nitrogen atmosphere
Isopropyl ester keeps recirculated cooling water, premixes and persistently stirs and vacuumize after continuing stirring 25 minutes 1h stopping, being filled with nitrogen in kettle
It discharges after gas to normal pressure, packs, obtain product.
1 organosilicon sealant the performance test results of table
Claims (10)
1. a kind of organosilicon sealant that fugitive constituent is controlled, it is characterised in that the parts by weight of its material component and each component are as follows:
In wherein α, alpha, omega-dihydroxy polydimethyl siloxane and dimethicone low molecular weight polycaprolactone content of siloxane be 100~
300ppm。
2. organosilicon sealant according to claim 1, it is characterised in that the α, alpha, omega-dihydroxy polydimethyl silicon oxygen
Viscosity of the alkane at 25 DEG C is 1500~80000mPas.
3. organosilicon sealant according to claim 1, it is characterised in that the dimethicone is viscous at 25 DEG C
Degree is 350~1000mPas.
4. organosilicon sealant according to claim 1, it is characterised in that the calcium carbonate is nm-class active calcium carbonate
Or one or both of powdered whiting.
5. organosilicon sealant according to claim 1, it is characterised in that the fumed silica is hydrophobic type, than
Surface area is 150~380m2/g。
6. organosilicon sealant according to claim 1, it is characterised in that the crosslinking agent is methyl orthosilicate, positive silicon
Acetoacetic ester, methyltrimethoxysilane, methyltriethoxysilane, vinyltrimethoxysilane, vinyl triethoxyl silicon
At least one of alkane, phenyltrimethoxysila,e or phenyl triethoxysilane.
7. organosilicon sealant according to claim 1, it is characterised in that the coupling agent be KH470, KH550,
At least one of KH560, KH570 or KH792.
8. organosilicon sealant according to claim 1, it is characterised in that the catalyst is isopropyl titanate, two
In (ethyl acetoacetate) titanium diisopropyl ester, bis- (acetylacetone,2,4-pentanedione) metatitanic acid diisopropyl esters or bis- (acetylacetone,2,4-pentanedione) metatitanic acid diisobutyl esters
One kind.
9. a kind of method for preparing organosilicon sealant as described in claim 1, the specific steps of which are as follows:
(1) first stearic acid modified calcium carbonate, carbon black and fumed silica are dried；
(2) then by α, alpha, omega-dihydroxy polydimethyl siloxane, dimethicone, calcium carbonate, carbon black and fumed silica add
Enter in blender, 2~4h is stirred and be dehydrated at 100~120 DEG C, -0.09~-0.1MPa, obtains uniformly mixed basic glue
Material；
(3) by the cooling addition reaction kettle of sizing, crosslinking agent is added, and stir and mix under recirculated cooling water and vacuum environment
It closes 10~15 minutes；
(4) coupling agent and catalyst is added under nitrogen atmosphere again, keeps recirculated cooling water, is stirred 20~40 minutes after premix；
(5) it reduces mixing speed and stirs and persistently vacuumize 1~2h stopping, discharging after being filled with nitrogen to normal pressure in kettle, pack, obtain
To product.
10. according to the method described in claim 9, it is characterized in that the mixing speed in step (3) and (4) is 600~800
Rev/min；Mixing speed in step (5) is 50~100 revs/min.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102206349A (en) * | 2011-04-23 | 2011-10-05 | 茂名市信翼化工有限公司 | Method for purifying alpha,omega-dihydroxy-polydimethylsiloxane |
| CN102277126A (en) * | 2011-06-28 | 2011-12-14 | 成都硅宝科技股份有限公司 | Single-component dealcholization-type silicon sealant used for automobile lamp and preparation method thereof |
| CN104877621A (en) * | 2015-06-04 | 2015-09-02 | 绵阳惠利电子材料有限公司 | Polyorganosilicone sealant used for vehicle lamp assembly and preparing method thereof |
-
2018
- 2018-12-24 CN CN201811578876.9A patent/CN109735297A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102206349A (en) * | 2011-04-23 | 2011-10-05 | 茂名市信翼化工有限公司 | Method for purifying alpha,omega-dihydroxy-polydimethylsiloxane |
| CN102277126A (en) * | 2011-06-28 | 2011-12-14 | 成都硅宝科技股份有限公司 | Single-component dealcholization-type silicon sealant used for automobile lamp and preparation method thereof |
| CN104877621A (en) * | 2015-06-04 | 2015-09-02 | 绵阳惠利电子材料有限公司 | Polyorganosilicone sealant used for vehicle lamp assembly and preparing method thereof |
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Application publication date: 20190510 |