CN103613930B - The preparation method of the dealcoholizing-type silicone seal of resistance to-100 DEG C of low temperature - Google Patents
The preparation method of the dealcoholizing-type silicone seal of resistance to-100 DEG C of low temperature Download PDFInfo
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- CN103613930B CN103613930B CN201310601318.0A CN201310601318A CN103613930B CN 103613930 B CN103613930 B CN 103613930B CN 201310601318 A CN201310601318 A CN 201310601318A CN 103613930 B CN103613930 B CN 103613930B
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- 238000002360 preparation method Methods 0.000 title claims abstract description 18
- 229920001296 polysiloxane Polymers 0.000 title claims abstract description 12
- 239000011259 mixed solution Substances 0.000 claims abstract description 36
- 238000003756 stirring Methods 0.000 claims abstract description 32
- 239000002994 raw material Substances 0.000 claims abstract description 21
- 239000006087 Silane Coupling Agent Substances 0.000 claims abstract description 14
- 125000002887 hydroxy group Chemical group [H]O* 0.000 claims abstract description 14
- -1 siloxanes Chemical class 0.000 claims abstract description 12
- 239000006096 absorbing agent Substances 0.000 claims abstract description 10
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 7
- 238000005728 strengthening Methods 0.000 claims abstract description 7
- 239000012467 final product Substances 0.000 claims abstract description 4
- FFUAGWLWBBFQJT-UHFFFAOYSA-N hexamethyldisilazane Chemical group C[Si](C)(C)N[Si](C)(C)C FFUAGWLWBBFQJT-UHFFFAOYSA-N 0.000 claims description 20
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 16
- 239000000203 mixture Substances 0.000 claims description 15
- DOIRQSBPFJWKBE-UHFFFAOYSA-N dibutyl phthalate Chemical compound CCCCOC(=O)C1=CC=CC=C1C(=O)OCCCC DOIRQSBPFJWKBE-UHFFFAOYSA-N 0.000 claims description 12
- 239000000463 material Substances 0.000 claims description 11
- 239000000377 silicon dioxide Substances 0.000 claims description 8
- UKLDJPRMSDWDSL-UHFFFAOYSA-L [dibutyl(dodecanoyloxy)stannyl] dodecanoate Chemical compound CCCCCCCCCCCC(=O)O[Sn](CCCC)(CCCC)OC(=O)CCCCCCCCCCC UKLDJPRMSDWDSL-UHFFFAOYSA-L 0.000 claims description 7
- 235000010290 biphenyl Nutrition 0.000 claims description 7
- KOVKEDGZABFDPF-UHFFFAOYSA-N n-(triethoxysilylmethyl)aniline Chemical compound CCO[Si](OCC)(OCC)CNC1=CC=CC=C1 KOVKEDGZABFDPF-UHFFFAOYSA-N 0.000 claims description 7
- ZUOUZKKEUPVFJK-UHFFFAOYSA-N phenylbenzene Natural products C1=CC=CC=C1C1=CC=CC=C1 ZUOUZKKEUPVFJK-UHFFFAOYSA-N 0.000 claims description 7
- WRIDQFICGBMAFQ-UHFFFAOYSA-N (E)-8-Octadecenoic acid Natural products CCCCCCCCCC=CCCCCCCC(O)=O WRIDQFICGBMAFQ-UHFFFAOYSA-N 0.000 claims description 6
- LQJBNNIYVWPHFW-UHFFFAOYSA-N 20:1omega9c fatty acid Natural products CCCCCCCCCCC=CCCCCCCCC(O)=O LQJBNNIYVWPHFW-UHFFFAOYSA-N 0.000 claims description 6
- QSBYPNXLFMSGKH-UHFFFAOYSA-N 9-Heptadecensaeure Natural products CCCCCCCC=CCCCCCCCC(O)=O QSBYPNXLFMSGKH-UHFFFAOYSA-N 0.000 claims description 6
- 239000005642 Oleic acid Substances 0.000 claims description 6
- ZQPPMHVWECSIRJ-UHFFFAOYSA-N Oleic acid Natural products CCCCCCCCC=CCCCCCCCC(O)=O ZQPPMHVWECSIRJ-UHFFFAOYSA-N 0.000 claims description 6
- 239000007822 coupling agent Substances 0.000 claims description 6
- QXJSBBXBKPUZAA-UHFFFAOYSA-N isooleic acid Natural products CCCCCCCC=CCCCCCCCCC(O)=O QXJSBBXBKPUZAA-UHFFFAOYSA-N 0.000 claims description 6
- VNBLTKHUCJLFSB-UHFFFAOYSA-N n-(trimethoxysilylmethyl)aniline Chemical compound CO[Si](OC)(OC)CNC1=CC=CC=C1 VNBLTKHUCJLFSB-UHFFFAOYSA-N 0.000 claims description 6
- ZQPPMHVWECSIRJ-KTKRTIGZSA-N oleic acid Chemical compound CCCCCCCC\C=C/CCCCCCCC(O)=O ZQPPMHVWECSIRJ-KTKRTIGZSA-N 0.000 claims description 6
- CPUDPFPXCZDNGI-UHFFFAOYSA-N triethoxy(methyl)silane Chemical compound CCO[Si](C)(OCC)OCC CPUDPFPXCZDNGI-UHFFFAOYSA-N 0.000 claims description 6
- 238000013019 agitation Methods 0.000 claims description 5
- 238000002156 mixing Methods 0.000 claims description 4
- SJECZPVISLOESU-UHFFFAOYSA-N 3-trimethoxysilylpropan-1-amine Chemical compound CO[Si](OC)(OC)CCCN SJECZPVISLOESU-UHFFFAOYSA-N 0.000 claims description 3
- XDLMVUHYZWKMMD-UHFFFAOYSA-N 3-trimethoxysilylpropyl 2-methylprop-2-enoate Chemical compound CO[Si](OC)(OC)CCCOC(=O)C(C)=C XDLMVUHYZWKMMD-UHFFFAOYSA-N 0.000 claims description 3
- 239000004593 Epoxy Substances 0.000 claims description 3
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 3
- QABCGOSYZHCPGN-UHFFFAOYSA-N chloro(dimethyl)silicon Chemical compound C[Si](C)Cl QABCGOSYZHCPGN-UHFFFAOYSA-N 0.000 claims description 3
- LIKFHECYJZWXFJ-UHFFFAOYSA-N dimethyldichlorosilane Chemical compound C[Si](C)(Cl)Cl LIKFHECYJZWXFJ-UHFFFAOYSA-N 0.000 claims description 3
- 150000002148 esters Chemical class 0.000 claims description 3
- 239000001301 oxygen Substances 0.000 claims description 3
- 229910052760 oxygen Inorganic materials 0.000 claims description 3
- 125000001436 propyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])[H] 0.000 claims description 3
- 230000008859 change Effects 0.000 claims description 2
- 125000006850 spacer group Chemical group 0.000 claims description 2
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 claims 1
- 238000000034 method Methods 0.000 abstract description 5
- 230000007704 transition Effects 0.000 abstract description 2
- 229920002379 silicone rubber Polymers 0.000 description 11
- 239000000047 product Substances 0.000 description 9
- 238000007789 sealing Methods 0.000 description 8
- 238000004519 manufacturing process Methods 0.000 description 4
- 239000004945 silicone rubber Substances 0.000 description 4
- 239000004590 silicone sealant Substances 0.000 description 4
- 238000005987 sulfurization reaction Methods 0.000 description 4
- 230000000694 effects Effects 0.000 description 3
- 230000009477 glass transition Effects 0.000 description 3
- 239000003566 sealing material 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
- 230000001070 adhesive effect Effects 0.000 description 2
- 238000002425 crystallisation Methods 0.000 description 2
- 230000008025 crystallization Effects 0.000 description 2
- 239000000565 sealant Substances 0.000 description 2
- 229920000260 silastic Polymers 0.000 description 2
- 238000003860 storage Methods 0.000 description 2
- UUEWCQRISZBELL-UHFFFAOYSA-N 3-trimethoxysilylpropane-1-thiol Chemical compound CO[Si](OC)(OC)CCCS UUEWCQRISZBELL-UHFFFAOYSA-N 0.000 description 1
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 1
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 1
- 239000005864 Sulphur Substances 0.000 description 1
- 230000032683 aging Effects 0.000 description 1
- 125000003545 alkoxy group Chemical group 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 238000004132 cross linking Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 239000004205 dimethyl polysiloxane Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000002708 enhancing effect Effects 0.000 description 1
- MOSXLDGILGBOSZ-UHFFFAOYSA-N ethenyl-methyl-phenylsilicon Chemical compound C=C[Si](C)C1=CC=CC=C1 MOSXLDGILGBOSZ-UHFFFAOYSA-N 0.000 description 1
- 238000011049 filling Methods 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 239000004973 liquid crystal related substance Substances 0.000 description 1
- 238000011068 loading method Methods 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 description 1
- 238000000465 moulding Methods 0.000 description 1
- HMMGMWAXVFQUOA-UHFFFAOYSA-N octamethylcyclotetrasiloxane Chemical compound C[Si]1(C)O[Si](C)(C)O[Si](C)(C)O[Si](C)(C)O1 HMMGMWAXVFQUOA-UHFFFAOYSA-N 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 238000004806 packaging method and process Methods 0.000 description 1
- 125000001997 phenyl group Chemical group [H]C1=C([H])C([H])=C(*)C([H])=C1[H] 0.000 description 1
- 229920000435 poly(dimethylsiloxane) Polymers 0.000 description 1
- 229910021420 polycrystalline silicon Inorganic materials 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 229920005591 polysilicon Polymers 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 150000003384 small molecules Chemical class 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 239000007858 starting material Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
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- Compositions Of Macromolecular Compounds (AREA)
- Sealing Material Composition (AREA)
Abstract
The present invention relates to a kind of preparation method of dealcoholizing-type silicone seal of resistance to-100 DEG C of low temperature, step is as follows: A, to α, omega end hydroxyl gathers in diphenyldimethyl siloxanes and adds moisture absorber, is uniformly mixed obtained mixed solution a; B, in mixed solution a, add strengthening agent, stir, obtained mixed solution b; C, mixed solution b is joined in planetary mixer, vacuumize, stir, obtained mixed solution c; D, under vacuum, in mixed solution c, add silane coupling agent, stir, then add catalyzer, continue to stir, obtained cast raw material; E, joined and install in the vulcanizing press of mould by cast raw material, room temperature lower open mouth is placed, and then matched moulds self cure, to obtain final product.Method preparation of the present invention makes the dealcoholizing-type silicone seal of resistance to-100 DEG C of low temperature obtained, second-order transition temperature Tg=-104 DEG C, and does not occur Tc.
Description
Technical field
The present invention relates to a kind of preparation method of dealcoholizing-type silicone seal of resistance to-100 DEG C of low temperature, belong to technical field of fine.
Background technology
Silicon rubber has good elasticity, insulativity and ageing-resistant performance, due to the molecular structure that it is special, makes it have excellent sealing effectiveness, is used widely.Usual silicone rubber has reliable sealing effectiveness in-50 DEG C ~ 280 DEG C temperature ranges.But under cryogenic, because the thermal motion of silicone sealant material Middle molecule reduces, molecule segment can become stiff and even freeze, and silicon rubber is followed the string, and causes sealing effectiveness difference even to lose sealing function.Therefore, when sealing material is applied to the equipment such as spacecraft, aircraft, ultra-deep freezer, cold district, pole engineering machinery and bullet train and region, the low temperature resistant silicon rubber guarantee safety of special preparation and the steady running of equipment must be adopted.This just requires that sealing material must possess excellent resistance to low temperature, makes it have low temperature resistant stability, just can reach corresponding seal request.
At present, the domestic organosilicon sealant kind used is a lot, major part adopts α, raw material production based on omega end hydroxyl polydimethylsiloxane, and in its molecular structure, side chain is all methyl, very regular, when envrionment temperature reaches about-50 DEG C, there will be crystallization, cause material hardens to become fragile, lose sealing function, range of application and field are restricted.
As Chinese patent literature CN102719216A(application number 201210236048.3) disclose the preparation method of a kind of liquid crystal coated optical cable matching gel stick.The α that the method utilizes low-temperature performance good, omega end hydroxyl gathers methyl vinyl phenyl silicon rubber or α, omega end hydroxyl polydimethyl di-ethyl siloxane is as material of main part, and adopt Nano filling enhancing silicone rubber adhesive to improve its mechanical property, according to the sulfuration mechanism of dealcoholized type room temperature vulcanized silicone rubber, prepare the room temperature vulcanized silastic adhesive that low-temperature performance is excellent, tripping force is moderate.
Summary of the invention
The present invention is directed to the deficiencies in the prior art, a kind of preparation method of dealcoholizing-type silicone seal of resistance to-100 DEG C of low temperature is provided.
Term explanation
1. dealcoholizing-type silicone seal: refer in the coupling agent molecule selected and contain alkoxyl group, when organosilicon material sulphur, discharge small molecular alcohol, rest part cross moulding.
2. resistance to low temperature: glass transition temperature Tg is lower, the high molecular polymer that crystallinity is less, resistance to low temperature is better.
3. resistance to-100 DEG C of low temperature: refer to that the Tg of macromolecular material is lower than-100 DEG C, and do not occur Tc.
4.D
4: octamethylcyclotetrasiloxane.
Technical solution of the present invention is as follows:
The preparation method of the dealcoholizing-type silicone seal of resistance to-100 DEG C of low temperature, step is as follows:
A, be that under the agitation condition of 25 ~ 90 revs/min, to the α of 60 ~ 80 weight parts, omega end hydroxyl gathers the moisture absorber adding 0.1 ~ 0.5 weight part in diphenyldimethyl siloxanes, is uniformly mixed 15 ~ 30 minutes, obtained mixed solution a in speed;
Described α, omega end hydroxyl gather diphenyldimethyl siloxanes range of viscosities be 2 × 10
3~ 1 × 10
5mPas;
Described moisture absorber is hexamethyldisilazane or isocyanic ester;
Add the strengthening agent of 10 ~ 25 weight parts in B, the mixed solution a that obtains to steps A, under the condition of 25 ~ 90 revs/min of stirring velocitys, stir 2 ~ 3.5 hours, obtained mixed solution b;
Described strengthening agent is that surface is hydrophobically modified, specific surface area is 80 ~ 250m
2the thermal silica of/g;
C, mixed solution b obtained for step B is joined in planetary mixer, be evacuated to 1 × 10
-3~ 10
-4pa, stirs 30 ~ 60 minutes with the speed of 20 ~ 70 revs/min, obtained mixed solution c;
D, under vacuum, in the mixed solution c that step C obtains, add the silane coupling agent of 2 ~ 7 weight parts, under the speed conditions of 20 ~ 70 revs/min, stir 15 ~ 30 minutes, then add the catalyzer of 2 ~ 7 weight parts, continue stirring 15 ~ 30 minutes, obtained cast raw material;
Described silane coupling agent is dealcoholizing-type coupling agent mixture;
E, the cast raw material obtained by step D join and install in the vulcanizing press of mould, and room temperature lower open mouth is placed 15 ~ 30 minutes, and then matched moulds self cure 24 ~ 120 hours, to obtain final product.Depending on spacer thickness difference, curing time also can respective change.
Preferred according to the present invention, in described steps A, α, the phenylbenzene silica chain link molar content scope that omega end hydroxyl gathers diphenyldimethyl siloxanes is 5% ~ 18%; Phenylbenzene silica chain link molar content is too low, the silicon rubber produced can be caused to occur crystalline polamer and do not have resistance to low temperature, and phenylbenzene silica chain link molar content is too high, Material synthesis difficulty, can cause high cost, not have actual production meaning.
Preferred according to the present invention, in described steps A, moisture absorber is hexamethyldisilazane.
Preferred according to the present invention, in described step B, strengthening agent is that surface is through hexamethyldisilazane, D
4or dimethyldichlorosilane(DMCS) hydrophobically modified, specific surface area is 80 ~ 250m
2the thermal silica of/g.This product is existing commercially available prod, as on sale in Cabot Co., Ltd of the U.S..
Preferred according to the present invention, in described step D, dealcoholizing-type coupling agent mixture is the mixing that materials two or more in anilinomethyl trimethoxy silane, anilinomethyl triethoxysilane, γ-aminopropyl-Trimethoxy silane, γ-(2,3-epoxy third oxygen) propyl trimethoxy silicane, γ-methacryloxypropyl trimethoxy silane and Union carbide A-162 presses any ratio; Further preferred silane coupling agent is the mixture of anilinomethyl trimethoxy silane, anilinomethyl triethoxysilane and Union carbide A-162 1.5:1.0:0.2 in mass ratio.This silane coupling agent proportioning determines raw material crosslinking degree, and proportioning is not right, and easily remaining free small molecules in silicon rubber, can form detrimentally affect to final product, finally can reduce low temperature resistant effect.
Preferred according to the present invention, in described step D, catalyzer is the mixing by any ratio of dibutyl tin laurate, dibutyl phthalate and oleic acid; Preferred further, catalyzer is dibutyl tin laurate, dibutyl phthalate and the oleic acid mixture by weight 1.0:4:5.This catalyst loading and proportioning determine silicon rubber self-vulcanizing speed, too fast or cross and all easily make silastic structure produce defect slowly, finally affect the low temperature resistant effect of product.
In the preparation method of above-mentioned resistance to-100 DEG C of low temperature polysilicon confidential paper, mold shape in step e can be O type, U-shaped, V-type, W type, X-type, Y type and square strip and circular strip etc., also can be certain thickness plate and die, this be all the routine selection of this area.
Beneficial effect
1, the present invention adopts the raw material being different from prior art, ensure that product molecule side chain contains two or more different groups, break the regular system of group, eliminate the basis that crystallization occurs, put in order by different proportioning raw materials, catalyzer and different groups, reduce the second-order transition temperature of material, eliminate Tc, reach low temperature resistant effect.The dealcoholizing-type silicone seal of obtained resistance to-100 DEG C of low temperature, glass transition temperature Tg=-104 DEG C, and there is not Tc.
2, product performance prepared by the method for the invention are reliable, expand the temperature resistant range of organosilicon sealant, overcome the weakness of common silicone seal, can meet envrionment temperature more than-100 DEG C time seal request, effectively meet aerospace industry, spacecraft, aircraft, naval vessel, ultra-deep freezer, the equipment such as cold district, pole engineering machinery and bullet train and region are to the demand of organosilicon sealing material, different moulds can be adopted to make the sealed strip of different shape respectively, sealing-ring and gasket seal, silicone rubber seal uses pressure: <3.0MPa, pad specification DN5 ~ DN400mm, greatly expand range of application.
3, the method for the invention simple process, starting material usage quantity is few, and production unit drops into low, does not have noise and exhaust gas emission, and the tankage of production can reclaiming, can not cause secondary pollution to environment, and product is convenient to store, transport, packaging and use.
Accompanying drawing explanation
Fig. 1 is dynamic thermomechanometry DMA spectrogram storage modulus-temperature curve and the out-of-phase modulus-temperature curve that embodiment 1 obtains product;
Wherein: M ' is storage modulus-temperature curve, M " is out-of-phase modulus-temperature curve;
Fig. 2 is dynamic thermomechanometry DMA spectrogram spillage of material coefficient (tan the δ)-temperature curve that embodiment 1 obtains product;
Embodiment
Followingly technical scheme of the present invention to be described further, but institute of the present invention protection domain is not limited only to this in conjunction with the embodiments.
Raw material sources
The surface used in embodiment through hexamethyldisilazane hydrophobically modified, specific surface area is 150 ~ 250m
2the thermal silica of/g can be bought from market, as: Cabot Co., Ltd of the U.S. is on sale;
α, omega end hydroxyl gathers diphenyldimethyl siloxanes and can buy from market, and Shanghai Resin Factory Co., Ltd. is on sale;
All raw materials such as silane coupling agent used, catalyzer are commercial products.
Embodiment 1
A preparation method for the dealcoholizing-type organosilicon O RunddichtringO of resistance to-100 DEG C of low temperature, step is as follows:
A, by 78 weight part α, omega end hydroxyl gathers diphenyldimethyl siloxanes (phenylbenzene silica chain link molar content is 9.3%) and puts into container, under the speed of 50 revs/min stir, add the hexamethyldisilazane of 0.2 weight part as moisture absorber, the time of being uniformly mixed is 30 minutes, obtained mixed solution a;
B, by 14 weight parts surfaces through hexamethyldisilazane hydrophobically modified, specific surface area is 200m
2the thermal silica of/g under agitation, slowly joins in the obtained mixed solution a of steps A, with the stirring velocity of 50 revs/min, stirs 2 hours, obtained mixed solution b, stand for standby use;
C, join in planetary mixer by mixed solution b obtained for step B, being evacuated to is 1 × 10
-3~ 10
-4pa, stirs 30 minutes with the speed of 30 revs/min, carries out degassed processed to raw material, obtained mixed solution c;
D, under vacuum, in the mixed solution c that step C obtains, add the silane coupling agent of 5 weight parts, stir 20 minutes, then add the catalyzer of 2.8 weight parts, continue stirring 20 minutes, obtained cast raw material;
Silane coupling agent is the mixture of anilinomethyl trimethoxy silane, anilinomethyl triethoxysilane and Union carbide A-162 1.5:1.0:0.2 in mass ratio;
Catalyzer is dibutyl tin laurate, dibutyl phthalate and the oleic acid mixture by weight 1.0:4:5;
E, the cast raw material obtained by step D join the vulcanizing press installing O type ring mould, room temperature lower open mouth places 20 minutes, make its surface cure, then matched moulds self cure, sulfuration 48 hours, the i.e. dealcoholizing-type organosilicon O RunddichtringO of get Nai-100 DEG C of low temperature, specification is DN5 ~ DN400mm.
Detect through dynamic thermomechanometry DMA spectrogram, as depicted in figs. 1 and 2, result shows that the glass transition temperature Tg of material is-104 DEG C to result, does not have Tc to occur.
Embodiment 2
A preparation method for the dealcoholizing-type organosilicon gasket of resistance to-100 DEG C of low temperature, step is as follows:
A, by 72 weight part α, omega end hydroxyl gathers diphenyldimethyl siloxanes (phenylbenzene silica chain link molar content is 9.7%) and puts into container, under the speed of 50 revs/min stir, add the isocyanic ester of 0.2 weight part as moisture absorber, the time of being uniformly mixed is 15 minutes, obtained mixed solution a;
B, by 20 weight part surface D
4hydrophobically modified, specific surface area is 150m
2the thermal silica of/g under agitation, slowly joins in the obtained mixed solution a of steps A, with the stirring velocity of 30 revs/min, stirs 3.5 hours, obtained mixed solution b, stand for standby use;
C, join in planetary mixer by mixed solution b obtained for step B, being evacuated to is 1 × 10
-3~ 10
-4pa, stirs 30 minutes with the speed of 30 revs/min, carries out degassed processed to raw material, obtained mixed solution c;
D, under vacuum, in the mixed solution c that step C obtains, add the silane coupling agent of 4 weight parts, stir 30 minutes, then add the catalyzer of 3.8 weight parts, continue stirring 30 minutes, obtained cast raw material;
Silane coupling agent is the mixture of anilinomethyl trimethoxy silane, γ-(2,3-epoxy third oxygen) propyl trimethoxy silicane, anilinomethyl triethoxysilane and γ-aminopropyl-Trimethoxy silane 1.5:0.3:1.0:0.5 in mass ratio;
Catalyzer is dibutyl tin laurate and the oleic acid mixture by weight 1.0:8;
E, the cast raw material obtained by step D join the vulcanizing press installing sealing gasket die, and room temperature lower open mouth places 30 minutes, makes its surface cure, then matched moulds self cure, sulfuration 60 hours, i.e. the dealcoholizing-type silicone sealant pad of get Nai-100 DEG C of low temperature, specification is DN5 ~ DN400mm.
Embodiment 3
A preparation method for the dealcoholizing-type silicone sealant block of resistance to-100 DEG C of low temperature, step is as follows:
A, by 66 weight part α, omega end hydroxyl gathers diphenyldimethyl siloxanes (phenylbenzene silica chain link molar content is 10.2%) and puts into container, under the speed of 50 revs/min stir, add the hexamethyldisilazane of 0.3 weight part as moisture absorber, the time of being uniformly mixed is 15 minutes, obtained mixed solution a;
B, by 24 weight parts surfaces dimethyldichlorosilane(DMCS) hydrophobically modified, specific surface area is 120m
2the thermal silica of/g under agitation, slowly joins in the obtained mixed solution a of steps A, with the stirring velocity of 30 revs/min, stirs 3 hours, obtained mixed solution b, stand for standby use;
C, join in planetary mixer by mixed solution b obtained for step B, being evacuated to is 1 × 10
-3~ 10
-4pa, stirs 30 minutes with the speed of 30 revs/min, carries out degassed processed to raw material, obtained mixed solution c;
D, under vacuum, in the mixed solution c that step C obtains, add the silane coupling agent of 4.5 weight parts, stir 20 minutes, then add the catalyzer of 5.2 weight parts, continue stirring 30 minutes, obtained cast raw material;
Silane coupling agent be γ-mercapto propyl-trimethoxysilane, the mixture of anilinomethyl triethoxysilane, γ-methacryloxypropyl trimethoxy silane and Union carbide A-162 1.5:1.0:0.2:0.2 in mass ratio;
Catalyzer is dibutyl tin laurate and the dibutyl phthalate mixture by weight 1.0:6;
E, the cast raw material obtained by step D join the vulcanizing press installing sealing gasket die, room temperature lower open mouth places 30 minutes, make its surface cure, then matched moulds self cure, sulfuration 120 hours, the i.e. dealcoholizing-type silicone sealant block of get Nai-100 DEG C of low temperature, sealing block thickness is specification 5 ~ 15mm.
After testing, the mechanical property of the dealcoholizing-type silicone seal product of resistance to-100 DEG C of low temperature that embodiment 1 ~ 3 is obtained is as shown in table 1:
Table 1
| Embodiment | Phenyl chain link (%) | Hardness (Shore A) | Tensile strength (MPa) | Elongation rate of tensile failure (%) |
| 1 | 9.3 | 32 | 1.76 | 185 |
| 2 | 9.7 | 33 | 1.83 | 186 |
| 3 | 10.2 | 36 | 1.87 | 191 |
Claims (5)
1. the preparation method of the dealcoholizing-type silicone seal of resistance to-100 DEG C of low temperature, it is characterized in that, step is as follows:
A, be that under the agitation condition of 25 ~ 90 revs/min, to the α of 60 ~ 80 weight parts, omega end hydroxyl gathers the moisture absorber adding 0.1 ~ 0.5 weight part in diphenyldimethyl siloxanes, is uniformly mixed 15 ~ 30 minutes, obtained mixed solution a in speed;
Described α, the range of viscosities that omega end hydroxyl gathers diphenyldimethyl siloxanes is: 2 × 10
3~ 1 × 10
5mPas; α, the phenylbenzene silica chain link molar content scope that omega end hydroxyl gathers diphenyldimethyl siloxanes is 5% ~ 18%;
Described moisture absorber is hexamethyldisilazane or isocyanic ester;
Add the strengthening agent of 10 ~ 25 weight parts in B, the mixed solution a that obtains to steps A, under the condition of 25 ~ 90 revs/min of stirring velocitys, stir 2 ~ 3.5 hours, obtained mixed solution b;
Described strengthening agent is that surface is hydrophobically modified, specific surface area is 80 ~ 250m
2the thermal silica of/g;
C, mixed solution b obtained for step B is joined in planetary mixer, be evacuated to 1 × 10
-3~ 10
-4pa, stirs 30 ~ 60 minutes with the speed of 20 ~ 70 revs/min, obtained mixed solution c;
D, under vacuum, in the mixed solution c that step C obtains, add the silane coupling agent of 2 ~ 7 weight parts, under the speed conditions of 20 ~ 70 revs/min, stir 15 ~ 30 minutes, then add the catalyzer of 2 ~ 7 weight parts, continue stirring 15 ~ 30 minutes, obtained cast raw material;
Described silane coupling agent is dealcoholizing-type coupling agent mixture; Dealcoholizing-type coupling agent mixture is the mixing that materials two or more in anilinomethyl trimethoxy silane, anilinomethyl triethoxysilane, γ-aminopropyl-Trimethoxy silane, γ-(2,3-epoxy third oxygen) propyl trimethoxy silicane, γ-methacryloxypropyl trimethoxy silane and Union carbide A-162 presses any ratio;
Described catalyzer is the mixing by any ratio of dibutyl tin laurate, dibutyl phthalate and oleic acid;
E, the cast raw material obtained by step D join and install in the vulcanizing press of mould, and room temperature lower open mouth is placed 15 ~ 30 minutes, and then matched moulds self cure 24 ~ 120 hours, to obtain final product, and depending on spacer thickness difference, curing time also can respective change.
2. preparation method as claimed in claim 1, it is characterized in that, in described steps A, moisture absorber is hexamethyldisilazane.
3. preparation method as claimed in claim 1, is characterized in that, in described step B, strengthening agent is that surface is through hexamethyldisilazane, D
4or dimethyldichlorosilane(DMCS) hydrophobically modified, specific surface area is 80 ~ 250m
2the thermal silica of/g.
4. preparation method as claimed in claim 1, it is characterized in that, in described step D, dealcoholizing-type coupling agent mixture is the mixture of anilinomethyl trimethoxy silane, anilinomethyl triethoxysilane and Union carbide A-162 1.5:1.0:0.2 in mass ratio.
5. preparation method as claimed in claim 1, is characterized in that, in described step D, catalyzer is dibutyl tin laurate, dibutyl phthalate and the oleic acid mixture by weight 1.0:4:5.
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| CN102719216A (en) * | 2012-07-09 | 2012-10-10 | 北京化工大学 | Preparation method of adhesive assorted with liquid crystal coated optical cable |
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| CN1482200A (en) * | 2003-05-15 | 2004-03-17 | 四川大学 | Optically clear room temperature curing silicone sealing compound and method for preparing same |
| CN102020852A (en) * | 2009-09-15 | 2011-04-20 | 信越化学工业株式会社 | Underfill composition and an optical semiconductor device |
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Denomination of invention: Preparation method of dealcoholized silicone seal resistant to - 100 degC low temperature Effective date of registration: 20211227 Granted publication date: 20151118 Pledgee: Weifang Bank Co.,Ltd. Linqu sub branch Pledgor: SHANDONG BAOLONGDA INDUSTRIAL GROUP CO.,LTD. Registration number: Y2021980016353 |
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