CN102559133B - Addition type single component organosilicon sealant and processing method thereof - Google Patents
Addition type single component organosilicon sealant and processing method thereof Download PDFInfo
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- CN102559133B CN102559133B CN201110439040.2A CN201110439040A CN102559133B CN 102559133 B CN102559133 B CN 102559133B CN 201110439040 A CN201110439040 A CN 201110439040A CN 102559133 B CN102559133 B CN 102559133B
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- 239000000565 sealant Substances 0.000 title claims abstract description 27
- 238000003672 processing method Methods 0.000 title abstract 3
- 239000000463 material Substances 0.000 claims abstract description 25
- 238000003756 stirring Methods 0.000 claims abstract description 22
- 229920002545 silicone oil Polymers 0.000 claims abstract description 19
- 239000000203 mixture Substances 0.000 claims abstract description 14
- 125000000391 vinyl group Chemical group [H]C([*])=C([H])[H] 0.000 claims abstract description 13
- 229920002554 vinyl polymer Polymers 0.000 claims abstract description 13
- -1 polydimethylsiloxane Polymers 0.000 claims abstract description 10
- 230000018044 dehydration Effects 0.000 claims abstract description 7
- 238000006297 dehydration reaction Methods 0.000 claims abstract description 7
- 239000004205 dimethyl polysiloxane Substances 0.000 claims abstract description 7
- 229920000435 poly(dimethylsiloxane) Polymers 0.000 claims abstract description 7
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 6
- 239000003112 inhibitor Substances 0.000 claims abstract description 6
- 238000010276 construction Methods 0.000 claims description 23
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 claims description 18
- 229910052739 hydrogen Inorganic materials 0.000 claims description 16
- 239000001257 hydrogen Substances 0.000 claims description 16
- 239000002253 acid Substances 0.000 claims description 15
- DSVRVHYFPPQFTI-UHFFFAOYSA-N bis(ethenyl)-methyl-trimethylsilyloxysilane;platinum Chemical compound [Pt].C[Si](C)(C)O[Si](C)(C=C)C=C DSVRVHYFPPQFTI-UHFFFAOYSA-N 0.000 claims description 13
- 239000011347 resin Substances 0.000 claims description 12
- 229920005989 resin Polymers 0.000 claims description 12
- 150000002431 hydrogen Chemical class 0.000 claims description 9
- 229910052697 platinum Inorganic materials 0.000 claims description 9
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 7
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 7
- 239000006229 carbon black Substances 0.000 claims description 7
- 230000007704 transition Effects 0.000 claims description 7
- VTYYLEPIZMXCLO-UHFFFAOYSA-L calcium carbonate Substances [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 claims description 6
- 229910000019 calcium carbonate Inorganic materials 0.000 claims description 6
- FFUAGWLWBBFQJT-UHFFFAOYSA-N hexamethyldisilazane Chemical compound C[Si](C)(C)N[Si](C)(C)C FFUAGWLWBBFQJT-UHFFFAOYSA-N 0.000 claims description 6
- 238000002360 preparation method Methods 0.000 claims description 6
- 238000011049 filling Methods 0.000 claims description 5
- 238000000034 method Methods 0.000 claims description 5
- LTEHWCSSIHAVOQ-UHFFFAOYSA-N tripropyl borate Chemical compound CCCOB(OCCC)OCCC LTEHWCSSIHAVOQ-UHFFFAOYSA-N 0.000 claims description 5
- ZDQWESQEGGJUCH-UHFFFAOYSA-N Diisopropyl adipate Chemical compound CC(C)OC(=O)CCCCC(=O)OC(C)C ZDQWESQEGGJUCH-UHFFFAOYSA-N 0.000 claims description 4
- WRQNANDWMGAFTP-UHFFFAOYSA-N Methylacetoacetic acid Chemical compound COC(=O)CC(C)=O WRQNANDWMGAFTP-UHFFFAOYSA-N 0.000 claims description 4
- FAHBNUUHRFUEAI-UHFFFAOYSA-M hydroxidooxidoaluminium Chemical compound O[Al]=O FAHBNUUHRFUEAI-UHFFFAOYSA-M 0.000 claims description 4
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 claims description 4
- 229920001296 polysiloxane Polymers 0.000 claims description 4
- BDCLDNALSPBWPQ-UHFFFAOYSA-N 3-oxohexanoic acid Chemical compound CCCC(=O)CC(O)=O BDCLDNALSPBWPQ-UHFFFAOYSA-N 0.000 claims description 3
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 claims description 3
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims description 3
- 125000005133 alkynyloxy group Chemical group 0.000 claims description 3
- 125000004177 diethyl group Chemical group [H]C([H])([H])C([H])([H])* 0.000 claims description 3
- YYLGKUPAFFKGRQ-UHFFFAOYSA-N dimethyldiethoxysilane Chemical compound CCO[Si](C)(C)OCC YYLGKUPAFFKGRQ-UHFFFAOYSA-N 0.000 claims description 3
- 238000007789 sealing Methods 0.000 claims description 3
- 229910000077 silane Inorganic materials 0.000 claims description 3
- 239000010936 titanium Substances 0.000 claims description 3
- 229910052719 titanium Inorganic materials 0.000 claims description 3
- KPUWHANPEXNPJT-UHFFFAOYSA-N disiloxane Chemical class [SiH3]O[SiH3] KPUWHANPEXNPJT-UHFFFAOYSA-N 0.000 claims description 2
- 150000002148 esters Chemical class 0.000 claims description 2
- GCSJLQSCSDMKTP-UHFFFAOYSA-N ethenyl(trimethyl)silane Chemical compound C[Si](C)(C)C=C GCSJLQSCSDMKTP-UHFFFAOYSA-N 0.000 claims description 2
- 125000002510 isobutoxy group Chemical group [H]C([H])([H])C([H])(C([H])([H])[H])C([H])([H])O* 0.000 claims description 2
- 239000002245 particle Substances 0.000 claims description 2
- 239000003292 glue Substances 0.000 claims 1
- 239000003054 catalyst Substances 0.000 abstract description 3
- 238000002156 mixing Methods 0.000 abstract description 3
- 238000006243 chemical reaction Methods 0.000 abstract 1
- 239000012763 reinforcing filler Substances 0.000 abstract 1
- 239000004590 silicone sealant Substances 0.000 abstract 1
- 238000004519 manufacturing process Methods 0.000 description 7
- 229920002379 silicone rubber Polymers 0.000 description 5
- 230000001070 adhesive effect Effects 0.000 description 4
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 3
- 239000004411 aluminium Substances 0.000 description 3
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 3
- 229910052782 aluminium Inorganic materials 0.000 description 3
- FWDBOZPQNFPOLF-UHFFFAOYSA-N ethenyl(triethoxy)silane Chemical compound CCO[Si](OCC)(OCC)C=C FWDBOZPQNFPOLF-UHFFFAOYSA-N 0.000 description 3
- 239000011521 glass Substances 0.000 description 3
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 2
- 239000000853 adhesive Substances 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- 238000004382 potting Methods 0.000 description 2
- 229910052710 silicon Inorganic materials 0.000 description 2
- 239000010703 silicon Substances 0.000 description 2
- 239000004945 silicone rubber Substances 0.000 description 2
- 238000003860 storage Methods 0.000 description 2
- UKRDPEFKFJNXQM-UHFFFAOYSA-N vinylsilane Chemical compound [SiH3]C=C UKRDPEFKFJNXQM-UHFFFAOYSA-N 0.000 description 2
- 239000004925 Acrylic resin Substances 0.000 description 1
- 229920000178 Acrylic resin Polymers 0.000 description 1
- NDHFYDKYYXSPFR-UHFFFAOYSA-N CC(C)CO[Ti] Chemical compound CC(C)CO[Ti] NDHFYDKYYXSPFR-UHFFFAOYSA-N 0.000 description 1
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- KWYHDKDOAIKMQN-UHFFFAOYSA-N N,N,N',N'-tetramethylethylenediamine Chemical compound CN(C)CCN(C)C KWYHDKDOAIKMQN-UHFFFAOYSA-N 0.000 description 1
- NIXOWILDQLNWCW-UHFFFAOYSA-N acrylic acid group Chemical group C(C=C)(=O)O NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 239000010949 copper Substances 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000000280 densification Methods 0.000 description 1
- 239000012153 distilled water Substances 0.000 description 1
- 229920001971 elastomer Polymers 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- JEIPFZHSYJVQDO-UHFFFAOYSA-N ferric oxide Chemical compound O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 description 1
- 238000009998 heat setting Methods 0.000 description 1
- 230000002209 hydrophobic effect Effects 0.000 description 1
- 238000005286 illumination Methods 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 150000001282 organosilanes Chemical class 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 239000012994 photoredox catalyst Substances 0.000 description 1
- 239000004417 polycarbonate Substances 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 230000033764 rhythmic process Effects 0.000 description 1
- 238000010008 shearing Methods 0.000 description 1
- 239000007858 starting material Substances 0.000 description 1
- 238000005987 sulfurization reaction Methods 0.000 description 1
- 238000004073 vulcanization Methods 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
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- Sealing Material Composition (AREA)
Abstract
The invention discloses an addition type single component organosilicon sealant and a processing method thereof. The processing method is characterized by subjecting, by mass, 100 parts of vinyl silicone oil, 1-250 parts of reinforcing fillers, 0.5-2 parts of structured control agents, 10-30 parts of alpha, omega-dimethyl polydimethylsiloxane to dehydration and blending for 120-240 minutes in a vacuum kneader at the temperature of 120 DEG C to 170 DEG C, under the vacuum degree of 0.06-0.099 million pascal to obtain basic materials; adding, by mass, 100 parts of the base materials, 1-4 parts of hydrosilicone oil, 0.5-5 parts of inhibitors into a reaction kettle with a blender and a thermometer, stirring the mixture for 10 minutes, adding, by mass, 0.2-3 parts of catalysts, 0.1-1.0 part of tackifier, stirring the mixture for 10-15 minutes under the vacuum degree of 0.08-0.099 million pascal, continuously stirring the mixture for 10-15 minutes, adding, by mass, 0.1-0.5 parts of tackifier, stirring the mixture for 10-20 minutes under the vacuum degree of 0.08-0.099 million pascal, and continuously stirring the mixture for 5-10 minutes under the vacuum degree of 0.08-0.099 million pascal to obtain the addition type single component silicone sealant.
Description
Technical field
The present invention relates to add-on type One Component Silicons Construction Sealant and manufacture method thereof, belong to polymeric material field.
Background technology
Because silicon rubber has excellent high and low temperature resistance, remarkable weather-resistant performance, good hydrophobic performance etc., be widely used in industries such as building, electronic apparatus, automobile, illuminations.
Fast development along with scientific and technological progress, society, requires all trades and professions to have higher production efficiency.Due to the self-vulcanizing of addition-type silicon rubber energy, can fast setting under heating condition.Thereby, in fast-developing intensive electronic apparatus, new energy field extensive application prospect.Two-component silicone rubber in use, owing to being subject to the impact of blending ratio and mixing uniformity, can cause the difference of performance.And condensed type single-component silicon rubber is owing to solidifying by steam, thereby exist complete set time of long problem.Chinese patent CN 100482761C discloses a kind of single-component room-temperature fast sulfidization dealcoholization type sealing rubber with silicone structure and manufacture method thereof, at room temperature high-speed vulcanization, but after its sulfuration thickness 24h, also can only reach 4.0mm; US Patent No. 4481341 discloses a kind of platinum catalyst of thermofixation organosilane composition, use the silicon composition of this catalyzer at 23 ℃, to deposit viscosity after 35 days and be increased to 95000mPas by 93000mPas, but it need to solidify at 175 ℃ of 20min, and some electronic devices and components may hold can't stand so high temperature; Chinese patent CN101280168A discloses a kind of single component additional organosilicon electronic potting adhesive, but it need to be heating and curing above at 130 ℃, and not mentioned its shelf-time; In US Patent No. 6140446, mention the organic silicon potting adhesive using after a kind of catalyzer, at 105 ℃ 5min solidify but duration of service at 25 ℃ 100h only.Therefore, developing a kind ofly at room temperature has compared with long storage life, and under middle high and low temperature, quick-setting add-on type one-component silicone rubber adapts to increasingly fast-developing social production rhythm, will become following a kind of trend.
Summary of the invention
The object of the invention is provides add-on type One Component Silicons Construction Sealant and manufacture method thereof for the deficiencies in the prior art, be characterized in that this add-on type One Component Silicons Construction Sealant has excellent adhesiveproperties to glass, aluminium etc., under (23 ± 2) ℃ condition, can store more than 6 months, after 6 months, extrudability still good, under 120 ℃ of conditions, 20min solidifies, fast setting in 60min under 80 ℃ of conditions, more than tensile strength reaches 3.5MPa, elongation at break reaches more than 310%, and aluminium, glass, PC etc. are had to bonds well.The adhering and sealing that can be used for electricity-saving lamp, LED light fixture, electronic apparatus etc., shortens the production cycle.
Object of the present invention is realized by following technical measures, and wherein said starting material umber, except specified otherwise, is mass fraction.
The starting raw material component of add-on type One Component Silicons Construction Sealant is:
Wherein said base-material is:
Containing hydrogen silicone oil hydrogen content is 0.3%～1.5%.
Inhibitor is that 3-methyl isophthalic acid-hexin base-3-alcohol, methyl three (methyl fourth alkynyloxy group) silane, vinyl silane tri-butyl peroxy, Tetramethyl Ethylene Diamine and structure are
at least one in many vinyl of n=0～24 polysiloxane wherein.
Tackifier are annular siloxane, and its structural formula is
in formula, R
1=-(CH
2)
2si (OCH
2cH
3)
3or---(CH
2)
2si (OCH
2)
3or
or-CH
3;
or-(CH
2)
2si (OCH
2cH
3)
3or---(CH
2)
2si (OCH
2)
3or-CH
3; Or structural formula is
in formula, R
3=-CH
2cH
2=CH
2or-(CH
2)
3si (OCH
3)
3; R
4=-(CH
2)
3si (OCH
3)
3) or CH
2=CHSi (OCH
2cH
2oCH
3)
3); At least one in tripropoxy-boron and two isobutoxy titaniums two (ethyl acetoacetic acid) or diethoxy diethyl etheric acid titanium complex or two (methyl aceto acetate) aluminic acid diisopropyl ester.
Catalyzer is that platinum-divinyl tetramethyl disiloxane title complex of 30～100 mass parts is added in the organic-silicon-modified acrylic resin ester of 100 mass parts, after organosilicon modified crylic acid resin film forming, with shredder, grind to form platinum-divinyl tetramethyl disiloxane title complex of the organosilicon modified crylic acid resin parcel of particle diameter≤10 μ m, wherein, in platinum-divinyl tetramethyl disiloxane title complex, the content of platinum is 10～50ppm.
For wrapping up the second-order transition temperature of the organosilicon modified crylic acid resin of platinum-divinyl tetramethyl disiloxane, it is 40～120 ℃.
The viscosity of vinyl silicone oil when temperature is 25 ℃ is 5000～50000mPas.
This reinforced filling is nano-calcium carbonate or white carbon black.
Antistructurizing agent is at least one in dimethyldimethoxysil,ne, dimethyldiethoxysilane, hexamethyldisilazane and vinyl trimethylsilane.
The preparation method of add-on type One Component Silicons Construction Sealant comprises the following steps:
(1) preparation of base-material
By vinyl silicone oil 100 mass parts, reinforced filling 1～250 mass parts, antistructurizing agent 0.5～2 mass parts, α, ω-dimethyl polydimethylsiloxane 10～30 mass parts, in vacuum kneader in 120～170 ℃ of temperature, vacuum tightness 0.06～0.099MPa, dehydration blend 120～240min obtains base-material;
(2) preparation of add-on type One Component Silicons Construction Sealant:
By base-material 100 mass parts, containing hydrogen silicone oil 1～4 mass parts, inhibitor 0.5～5 mass parts, add with stirrer, in the reactor of thermometer, stir 10min, add again catalyzer 0.2～3 mass parts, tackifier 0.1～1.0 mass parts, stirs 10～15min, at vacuum tightness 0.08～0.099MPa, continues to stir 10～15min, add again tackifier 0.1～0.5 mass parts, at vacuum tightness 0.08～0.099MPa, continue to stir 10～20min, then under vacuum tightness 0.08～0.099MPa, continue to stir 5～10min, obtain single component additional organosilicon seal gum.
Performance test:
(1) press GB/T 531.1-2008 test shore hardness;
(2) press GB/T 528-2009 test elongation at break and breaking tenacity;
(3) according to standard GB/T7124-2008 test shearing resistance;
(4) according to standard GB/T13477, the 3rd partial test is extrudability, and spout is extruded aperture 6mm, pressure (0.34 ± 0.2) MPa;
(5) according to the gel time under standard GB 13477 test differing tempss.
Test result is as shown in Table 1 below.Result shows: by not organosilicon sealant and the relatively discovery of add-on type One Component Silicons Construction Sealant made in accordance with the present invention made in accordance with the present invention, add-on type One Component Silicons Construction Sealant prepared by the present invention, have at (23 ± 2) ℃ and have longer period of storage, middle high temperature rapid curing, compared with advantages such as high tensile and elongation at breaks, to aluminium, glass,, the material binding power such as copper, PC is good, the densification electronic apparatus industry and the industrial production that are suitable for increasingly developing.
The present invention has the following advantages:
1. in base-material, add antistructurizing agent and reinforced filling, make more than add-on type One Component Silicons Construction Sealant intensity reaches 3.5MPa, elongation at break reaches more than 310%, can bear certain stress and STRESS VARIATION.
2. by use second-order transition temperature, organosilicon modified crylic acid resin parcel platinum catalyst and the inhibitor at 40～120 ℃ is used in conjunction with in the present invention, make add-on type One Component Silicons Construction Sealant have more than 6 months shelf liveves at (23 ± 2) ℃, fast setting at 80～120 ℃, in intensive electronic enterprises is produced, application can be saved time, be enhanced productivity.
3. by directly add tackifier in add-on type One Component Silicons Construction Sealant, make add-on type One Component Silicons Construction Sealant itself there is remarkable adhesive property to base material, do not need to use in use primary coat, easy to use.
Embodiment
Below by the embodiment description concrete to the present invention; be necessary to be pointed out that at this following examples are only used to further illustrate the present invention; can not be interpreted as limiting the scope of the invention, the person skilled in the art in this field can content according to the present invention do some nonessential improvement and adjustment.
Embodiment 1: by vinyl silicone oil 100 mass parts that are 50000mPas in 25 ℃ of viscosity of temperature, white carbon black 40 mass parts add in vacuum kneader, α, ω-dimethyl polydimethylsiloxane 30 mass parts, add hexamethyldisilazane 2 mass parts, under normal temperature, mediate 30min, add distilled water 0.5 mass parts, mediate after 30min, in 170 ℃ of temperature, vacuum tightness 0.06MPa, vacuumizes 240min and obtains base-material.Containing hydrogen silicone oil 4 mass parts that are 0.3% by hydrogen content, 2-methyl-3-butynyl-2 alcohol 5 mass parts add stirrer and 100 mass parts base-materials to be uniformly mixed 10min, then add tripropoxy-boron 1 mass parts, CH
2=CHSi (OCH
2cH
2oCH
3)
30.3 mass parts, is uniformly mixed after 10min; Platinum-divinyl tetramethyl disiloxane title complex 0.2 mass parts that the platinum content that is the organosilicon modified crylic acid resin parcel of 40 ℃ by second-order transition temperature is 50ppm, two (methyl aceto acetate) aluminic acid diisopropyl ester, 0.5 mass parts, keep vacuum tightness to stir 20min at 0.099MPa, under vacuum tightness 0.099MPa, continue to vacuumize stirring 10min, obtain add-on type One Component Silicons Construction Sealant, the test result details of product performance are shown in Table 1.
Embodiment 2: by vinyl silicone oil 100 mass parts that viscosity is 5000mPas at 25 ℃ of temperature, nano-calcium carbonate 250 mass parts, α, ω-dimethyl polydimethylsiloxane 10 mass parts, white carbon black 1 mass parts, dimethyldiethoxysilane 0.5 mass parts, in 120 ℃ of temperature, vacuum tightness 0.099MPa dehydration blend 120min obtains base-material.Containing hydrogen silicone oil 1 mass parts that is 1.5% by hydrogen content, methyl three (methyl fourth alkynyloxy group) silane 0.5 mass parts, vinyl silane tri-butyl peroxy 0.1 mass parts, structural formula is
tackifier 0.15 mass parts, add in stirrer and 100 mass parts base-materials are uniformly mixed 10min, adding second-order transition temperature is platinum-divinyl tetramethyl disiloxane title complex 0.5 mass parts that the platinum content of the organosilicon modified crylic acid resin parcel of 120 ℃ is 50ppm, diethoxy diethyl etheric acid titanium complex 0.05 mass parts, keep vacuum tightness to be uniformly mixed 10min at 0.06MPa, under vacuum tightness 0.06MPa, continue to find time to stir 5min, obtain add-on type One Component Silicons Construction Sealant, the test result details of product performance are shown in Table 1.
Embodiment 3: by the vinyl silicone oil of 25 ℃ of viscosity 30000mPas, 100 mass parts, by nano-calcium carbonate 150 mass parts, white carbon black 15 mass parts, α, ω-dimethyl polydimethylsiloxane 20 mass parts, vinyltriethoxysilane 1 mass parts, add in vacuum kneader, in 150 ℃ of temperature, vacuum tightness 0.08MPa, dehydration blend 180min obtains base-material.Containing hydrogen silicone oil 3 mass parts that are 0.5% by hydrogen content, Tetramethyl Ethylene Diamine 0.1 mass parts, 2-methyl-3-butynyl-2 alcohol 0.6 mass parts, structural formula is
tackifier 0.5 mass parts, tripropoxy-boron 0.2 mass parts, add in stirrer and be uniformly mixed 10min with 100 mass parts base-materials, adding the platinum content of the organosilicon modified crylic acid resin parcel of 75 ℃ of second-order transition temperatures is 30ppm platinum-divinyl tetramethyl disiloxane title complex 0.2 mass parts again, two isobutoxy titanium two (ethyl acetoacetic acid) 0.1 mass parts, keep vacuum tightness to be uniformly mixed 15min at 0.08MPa, under vacuum tightness 0.08MPa, continue to vacuumize stirring 8min, obtain add-on type One Component Silicons Construction Sealant, the test result details of product performance are shown in Table 1.
Embodiment 4: by the vinyl silicone oil of 25 ℃ of viscosity 20000mPas, 100 mass parts, add nano-calcium carbonate 100 mass parts, white carbon black 20 mass parts, α, ω-dimethyl polydimethylsiloxane 20 mass parts, vinyltriethoxysilane 1 mass parts, in 150 ℃ of temperature, vacuum tightness 0.09MPa, dehydration blend 200min obtains base-material.Containing hydrogen silicone oil 4 mass parts that are 0.5% by hydrogen content, vinyl silane tri-butyl peroxy 0.5 mass parts, structural formula is
many vinyl polysiloxane 0.5 mass parts and 100 mass parts base-materials in stirrer, stir after 10min, add structural formula to be
tackifier 0.6 mass parts, tripropoxy-boron tackifier 0.15 mass parts is uniformly mixed 10min; Adding second-order transition temperature is platinum-divinyl tetramethyl disiloxane title complex 3 mass parts that the platinum content of the organosilicon modified crylic acid resin parcel of 60 ℃ is 10ppm again, two (methyl aceto acetate) aluminic acid diisopropyl ester, 0.2 mass parts, remaining on vacuum tightness 0.09MPa is uniformly mixed after 20min, under vacuum tightness 0.09MPa, continue to find time to stir 10min, obtain add-on type One Component Silicons Construction Sealant, the test result details of product performance are shown in Table 1.
Comparative example 1: will in temperature be vinyl silicone oil 100 mass parts that at 25 ℃, viscosity is 20000mPas, add nano-calcium carbonate 200 mass parts to add in vacuum kneader, white carbon black 10 mass parts, in 150 ℃ of temperature, under vacuum tightness 0.099MPa, dehydration blend 100min obtains base-material.Containing hydrogen silicone oil 4 mass parts that are 0.5% by hydrogen content, 2-methyl-3-butynyl-2 alcohol 8 mass parts, vinyltriethoxysilane 0.7 mass parts adds in stirrer and 100 mass parts base-materials are uniformly mixed 30min, platinum-divinyl tetramethyl disiloxane title complex 0.4 mass parts that is 30ppm by platinum content adds stirrer and 100 mass parts base-materials to be evacuated to vacuum tightness 0.09MPa to be uniformly mixed 20min, keep vacuum tightness to stir 5min at 0.08MPa, obtain add-on type One Component Silicons Construction Sealant.
Table 1
Claims (5)
1. add-on type One Component Silicons Construction Sealant, is characterized in that the feed composition of sealing glue is counted by following mass parts:
(1) wherein said base-material is:
Wherein, containing hydrogen silicone oil hydrogen content is 0.3%～1.5%; Inhibitor is that 3-methyl isophthalic acid-hexin base-3-alcohol, methyl three (methyl fourth alkynyloxy group) silane, vinyl silane tri-butyl peroxy, Tetramethyl Ethylene Diamine and structure are
at least one in many vinyl of n=0～24 polysiloxane wherein; Tackifier are annular siloxane, and its structural formula is
in formula, R
1=-(CH
2)
2si (OCH
2cH
3)
3or-(CH
2)
2si (OCH
2)
3or
or-CH
3;
or-(CH
2)
2si (OCH
2cH
3)
3or-(CH
2)
2si (OCH
2)
3or-CH
3; Or structural formula is
in formula, R
3=-CH
2cH
2=CH
2or-(CH
2)
3si (OCH
3)
3; R
4=-(CH
2)
3si (OCH
3)
3) or CH2=CHSi (OCH
2cH
2oCH
3)
3); At least one in tripropoxy-boron and two isobutoxy titaniums two (ethyl acetoacetic acid) or diethoxy diethyl etheric acid titanium complex or two (methyl aceto acetate) aluminic acid diisopropyl ester; Catalyzer is that platinum-divinyl tetramethyl disiloxane title complex of 30～100 mass parts is added in 100 mass parts organosilicon modified crylic acid resin esters, after organosilicon modified crylic acid resin film forming, with shredder, grind to form platinum-divinyl tetramethyl disiloxane title complex of the organosilicon modified crylic acid resin parcel of particle diameter≤10 μ m, wherein, in platinum-divinyl tetramethyl disiloxane title complex, the content of platinum is 10～50ppm; The second-order transition temperature that is used for wrapping up the organosilicon modified crylic acid resin of platinum-divinyl tetramethyl disiloxane is 40～120 ℃.
2. according to add-on type One Component Silicons Construction Sealant described in claim 1, it is characterized in that the viscosity of vinyl silicone oil when temperature is 25 ℃ is 5000～50000mPas.
3. according to add-on type list group organosilicon sealant described in claim 1, it is characterized in that this reinforced filling is nano-calcium carbonate or white carbon black.
4. according to add-on type One Component Silicons Construction Sealant described in claim 1, it is characterized in that antistructurizing agent is at least one in dimethyldimethoxysil,ne, dimethyldiethoxysilane, hexamethyldisilazane and vinyl trimethylsilane.
5. according to the preparation method of the described add-on type One Component Silicons Construction Sealant of one of claim 1～4, it is characterized in that the method comprises the following steps:
(1) preparation of base-material
By vinyl silicone oil 100 mass parts; reinforced filling 1～250 mass parts; antistructurizing agent 0.5～2 mass parts; α; ω-dimethyl polydimethylsiloxane 10～30 mass parts; in vacuum kneader in 120～170 ℃ of temperature, vacuum tightness 0.06～0.099MPa, dehydration blend 120～240min obtains base-material;
(2) preparation of add-on type One Component Silicons Construction Sealant:
By base-material 100 mass parts, containing hydrogen silicone oil 1～4 mass parts, inhibitor 0.5～5 mass parts, add with stirrer, in the reactor of thermometer, stir 10min, add again catalyzer 0.2～3 mass parts, tackifier 0.1～1.0 mass parts, stirs 10～15min, at vacuum tightness 0.08～0.099MPa, continues to stir 10～15min, add again tackifier 0.1～0.5 mass parts, at vacuum tightness 0.08～0.099MPa, continue to stir 10～20min, then under vacuum tightness 0.08～0.099MPa, continue to stir 5～10min, obtain single component additional organosilicon seal gum.
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| CN104448393B (en) * | 2013-09-23 | 2018-08-28 | 浙江新安化工集团股份有限公司 | Platiniferous fire retardant, room temperature vulcanized silicone rubber and preparation method thereof |
| CN106978104B (en) * | 2017-04-28 | 2019-05-17 | 深圳天鼎新材料有限公司 | Filler composition, the box dam glue comprising it, preparation method and application for box dam glue |
| CN107619656A (en) * | 2017-09-14 | 2018-01-23 | 佛山市天宝利硅工程科技有限公司 | A kind of method for packing of organic silicon rubber adhesive and electric-device housing |
| CN107936911A (en) * | 2017-11-17 | 2018-04-20 | 厦门安耐伟业新材料有限公司 | Organosilicon sealant and preparation method thereof |
| CN108728037A (en) * | 2018-05-11 | 2018-11-02 | 广州市联中电子科技有限公司 | A kind of adhesive and its manufacturing method increasing LED light module brightness |
| CN109504340B (en) * | 2018-11-20 | 2021-02-09 | 烟台德邦科技股份有限公司 | High-strength organic silicon heat-conducting sealant and preparation method thereof |
| CN111440591A (en) * | 2019-01-16 | 2020-07-24 | 北京氦舶科技有限责任公司 | Organosilicon conductive adhesive and preparation method thereof |
| CN109940930A (en) * | 2019-04-12 | 2019-06-28 | 福建宝利特科技股份有限公司 | A kind of reflective organosilicon synthetic leather and preparation method thereof |
| CN112111222A (en) * | 2020-09-10 | 2020-12-22 | 江苏天辰新材料股份有限公司 | Double-component addition type silicone rubber for priming-free polyamide base material and preparation method thereof |
| CN112226197B (en) * | 2020-09-17 | 2022-04-22 | 重庆重交再生资源开发股份有限公司 | Modified silicone sealant for treating asphalt pavement cracks and preparation method thereof |
| CN112280523A (en) * | 2020-09-21 | 2021-01-29 | 湖北平安电工材料有限公司 | Process for prolonging gelling time of hard mica plate adhesive and adhesive |
| CN113621138B (en) * | 2021-08-10 | 2022-10-21 | 湖北兴瑞硅材料有限公司 | Claw-type polyvinyl silicone oil and preparation method thereof |
| CN114574153A (en) * | 2022-03-09 | 2022-06-03 | 苏州艾迪亨斯胶粘技术有限公司 | Organosilicon sealant and preparation method thereof |
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| JP4648011B2 (en) * | 2005-01-13 | 2011-03-09 | 信越化学工業株式会社 | Silicone adhesive composition containing no aromatic solvent and adhesive tape, sheet or label coated with the same |
| JP2011137104A (en) * | 2009-12-28 | 2011-07-14 | Omron Corp | Silicone resin composition and utilization of the same |
| CN101787256A (en) * | 2009-12-30 | 2010-07-28 | 北京天山新材料技术有限责任公司 | Addition type silicone adhesive composition and preparation method thereof |
| CN102093839B (en) * | 2010-12-28 | 2015-08-26 | 成都硅宝科技股份有限公司 | A kind of add-on type joint sealant for aerogenerator and manufacture method thereof |
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Denomination of invention: Addition molding single component silicone sealant and its manufacturing method Granted publication date: 20140319 Pledgee: Chengdu Rural Commercial Bank Co.,Ltd. Wuhou Branch Pledgor: CHENGDU GUIBAO SCIENCE & TECHNOLOGY Co.,Ltd. Registration number: Y2024510000103 |