CN113980640A - Bi-component silicone hollow glass sealant B component and preparation method thereof - Google Patents
Bi-component silicone hollow glass sealant B component and preparation method thereof Download PDFInfo
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- CN113980640A CN113980640A CN202111406099.1A CN202111406099A CN113980640A CN 113980640 A CN113980640 A CN 113980640A CN 202111406099 A CN202111406099 A CN 202111406099A CN 113980640 A CN113980640 A CN 113980640A
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- 239000000565 sealant Substances 0.000 title claims abstract description 37
- 239000011521 glass Substances 0.000 title claims abstract description 36
- 229920001296 polysiloxane Polymers 0.000 title claims abstract description 34
- 238000002360 preparation method Methods 0.000 title abstract description 14
- 239000007822 coupling agent Substances 0.000 claims abstract description 43
- 239000011324 bead Substances 0.000 claims abstract description 34
- 238000000227 grinding Methods 0.000 claims abstract description 27
- 238000002156 mixing Methods 0.000 claims abstract description 25
- 239000000945 filler Substances 0.000 claims abstract description 24
- 239000004014 plasticizer Substances 0.000 claims abstract description 23
- 239000003054 catalyst Substances 0.000 claims abstract description 22
- 239000006229 carbon black Substances 0.000 claims abstract description 14
- QQQSFSZALRVCSZ-UHFFFAOYSA-N triethoxysilane Chemical compound CCO[SiH](OCC)OCC QQQSFSZALRVCSZ-UHFFFAOYSA-N 0.000 claims abstract description 13
- UKLDJPRMSDWDSL-UHFFFAOYSA-L [dibutyl(dodecanoyloxy)stannyl] dodecanoate Chemical group CCCCCCCCCCCC(=O)O[Sn](CCCC)(CCCC)OC(=O)CCCCCCCCCCC UKLDJPRMSDWDSL-UHFFFAOYSA-L 0.000 claims abstract description 8
- 239000012975 dibutyltin dilaurate Substances 0.000 claims abstract description 8
- 125000000118 dimethyl group Chemical group [H]C([H])([H])* 0.000 claims abstract description 8
- 229920002545 silicone oil Polymers 0.000 claims abstract description 8
- 239000000203 mixture Substances 0.000 claims abstract description 6
- 230000001681 protective effect Effects 0.000 claims abstract description 4
- WYTZZXDRDKSJID-UHFFFAOYSA-N (3-aminopropyl)triethoxysilane Chemical compound CCO[Si](OCC)(OCC)CCCN WYTZZXDRDKSJID-UHFFFAOYSA-N 0.000 claims abstract description 3
- BPSIOYPQMFLKFR-UHFFFAOYSA-N trimethoxy-[3-(oxiran-2-ylmethoxy)propyl]silane Chemical compound CO[Si](OC)(OC)CCCOCC1CO1 BPSIOYPQMFLKFR-UHFFFAOYSA-N 0.000 claims abstract description 3
- 239000000463 material Substances 0.000 claims description 43
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 38
- 238000010296 bead milling Methods 0.000 claims description 25
- 238000003756 stirring Methods 0.000 claims description 20
- 229910052757 nitrogen Inorganic materials 0.000 claims description 19
- 238000007599 discharging Methods 0.000 claims description 18
- 238000000034 method Methods 0.000 claims description 17
- 230000008569 process Effects 0.000 claims description 11
- 238000004806 packaging method and process Methods 0.000 claims description 10
- 238000007789 sealing Methods 0.000 claims description 10
- 238000005303 weighing Methods 0.000 claims description 10
- 238000011049 filling Methods 0.000 claims description 9
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 claims 2
- 239000002131 composite material Substances 0.000 abstract 1
- 231100000252 nontoxic Toxicity 0.000 abstract 1
- 230000003000 nontoxic effect Effects 0.000 abstract 1
- 239000002994 raw material Substances 0.000 abstract 1
- 239000000758 substrate Substances 0.000 abstract 1
- RVTZCBVAJQQJTK-UHFFFAOYSA-N oxygen(2-);zirconium(4+) Chemical compound [O-2].[O-2].[Zr+4] RVTZCBVAJQQJTK-UHFFFAOYSA-N 0.000 description 8
- 229910001928 zirconium oxide Inorganic materials 0.000 description 8
- 238000010276 construction Methods 0.000 description 6
- 238000001514 detection method Methods 0.000 description 6
- 238000004519 manufacturing process Methods 0.000 description 6
- 230000009286 beneficial effect Effects 0.000 description 2
- 238000004132 cross linking Methods 0.000 description 2
- AMTWCFIAVKBGOD-UHFFFAOYSA-N dioxosilane;methoxy-dimethyl-trimethylsilyloxysilane Chemical compound O=[Si]=O.CO[Si](C)(C)O[Si](C)(C)C AMTWCFIAVKBGOD-UHFFFAOYSA-N 0.000 description 2
- 239000011344 liquid material Substances 0.000 description 2
- 229940083037 simethicone Drugs 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- 229910000831 Steel Inorganic materials 0.000 description 1
- 230000004075 alteration Effects 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- 239000004566 building material Substances 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 238000009833 condensation Methods 0.000 description 1
- 230000005494 condensation Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000018044 dehydration Effects 0.000 description 1
- 238000006297 dehydration reaction Methods 0.000 description 1
- 229940008099 dimethicone Drugs 0.000 description 1
- 239000004205 dimethyl polysiloxane Substances 0.000 description 1
- 235000013870 dimethyl polysiloxane Nutrition 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 229920001971 elastomer Polymers 0.000 description 1
- 239000000806 elastomer Substances 0.000 description 1
- 238000001125 extrusion Methods 0.000 description 1
- 239000005329 float glass Substances 0.000 description 1
- 239000012530 fluid Substances 0.000 description 1
- 239000003292 glue Substances 0.000 description 1
- 230000007062 hydrolysis Effects 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
- 238000003801 milling Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 229920000435 poly(dimethylsiloxane) Polymers 0.000 description 1
- 230000002940 repellent Effects 0.000 description 1
- 239000005871 repellent Substances 0.000 description 1
- 238000005096 rolling process Methods 0.000 description 1
- 238000007665 sagging Methods 0.000 description 1
- 239000003566 sealing material Substances 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 239000004590 silicone sealant Substances 0.000 description 1
- 239000010959 steel Substances 0.000 description 1
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 description 1
- 229910052721 tungsten Inorganic materials 0.000 description 1
- 239000010937 tungsten Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J183/00—Adhesives based on macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon, with or without sulfur, nitrogen, oxygen, or carbon only; Adhesives based on derivatives of such polymers
- C09J183/04—Polysiloxanes
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
- C09J11/02—Non-macromolecular additives
- C09J11/04—Non-macromolecular additives inorganic
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
- C09J11/02—Non-macromolecular additives
- C09J11/06—Non-macromolecular additives organic
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Inorganic Chemistry (AREA)
- Sealing Material Composition (AREA)
- Compositions Of Macromolecular Compounds (AREA)
Abstract
The invention discloses a bi-component silicone hollow glass sealant B component and a preparation method thereof, wherein the B component comprises the following components in parts by weight: the composite material comprises polymethyl triethoxy silane, a filler, a plasticizer, a coupling agent I, a coupling agent II and a catalyst, wherein the filler is carbon black, the plasticizer is dimethyl silicone oil, the coupling agent I is gamma-aminopropyl triethoxy silane, the coupling agent II is gamma- (2, 3-epoxypropoxy) propyl trimethoxy silane, and the catalyst is dibutyltin dilaurate. When the hollow glass sealant is prepared specifically, the raw materials are uniformly mixed by a planetary mixer, the mixing is carried out in a protective atmosphere, then the mixture is subjected to bead grinding, and finally the component B is obtained, is mixed with the component A of the double-component silicone hollow glass sealant, has good bonding broad spectrum, is neutral-curing, is nontoxic and harmless, and is suitable for bonding of hollow glass sealants of various substrates.
Description
Technical Field
The invention relates to the technical field of silicone sealant production, in particular to a component B of a two-component silicone hollow glass sealant and a preparation method thereof.
Background
In modern building materials, environment-friendly materials are more and more widely used, and the bi-component silicone hollow glass sealant is widely used as a sealing material in door and window and curtain wall engineering. The traditional B component production process uses a three-roller machine for production, and the production mode is characterized in that: not only the production efficiency is low, but also the materials can be exposed in the air to absorb moisture in the manufacturing process to cause hydrolysis, thereby influencing the product quality.
Disclosure of Invention
The invention aims to overcome the defects and provide the component B of the double-component silicone hollow glass sealant and the preparation method thereof, so that the product has the advantages of refined particles and proper viscosity, and is beneficial to improving the product quality.
In order to solve the technical problems, the invention adopts the technical scheme that: a two-component silicone hollow glass sealant B component comprises the following components in parts by weight: 20-40 parts of polymethyl triethoxy silane, 10-30 parts of filler, 30-50 parts of plasticizer, 10-15 parts of coupling agent I, 5-10 parts of coupling agent II and 1-3 parts of catalyst.
Further, the content of the polymethyltriethoxysilane is 85-95%.
Further, the filler is carbon black, and the specific surface area of the carbon black is 110-130m2/g。
Further, the plasticizer is dimethyl silicone oil, and the viscosity is 330-370 mPa.s.
Further, the coupling agent I is gamma-aminopropyltriethoxysilane; the coupling agent II is gamma- (2, 3-epoxypropoxy) propyl trimethoxy silane; the catalyst was dibutyltin dilaurate.
The invention also relates to a method for preparing the component B of the two-component silicone hollow glass sealant, which comprises the following steps:
s1, weighing the polymethyltriethoxysilane, the plasticizer, the coupling agent I, the coupling agent II and the catalyst according to the proportion, uniformly mixing under a protective atmosphere, adding the filler, and uniformly mixing;
s2, stirring for 20-30 minutes in a vacuum state, stopping the vacuum pump, and filling nitrogen to 0.01-0.02 MPa;
and S3, transferring the material in the S2 to a bead mill for bead milling under the pressure of 0.1-0.3MPa and at the temperature of 30-50 ℃ for 5-10 minutes, discharging after the bead milling is finished, and sealing and packaging to obtain the component B of the bi-component silicone hollow glass sealant.
Further, the mixing device in S1 is a planetary mixer, the temperature is controlled at 40-60 ℃ during the mixing process, the mixture is stirred for 5-10 minutes in a nitrogen environment, and the mixture is stirred for 5-10 minutes after the filler is added.
Further, the pressure in S2 was-0.085 to-0.095 MPa.
Furthermore, in the S3 bead grinding, the used grinding beads have the diameter of 2-3mm and are made of zirconium oxide.
Further, the temperature is controlled to be 10-30 ℃ when discharging in S3.
The invention has the beneficial effects that:
(1) in the component B of the double-component silicone hollow glass sealant provided by the invention, the polymethyltriethoxysilane and the 107 glue in the component A are subjected to condensation crosslinking reaction at room temperature under the catalysis of a catalyst dibutyltin dilaurate, so that micromolecules are removed, and the elastomer with a three-dimensional network crosslinking structure is obtained. The viscosity of the plasticizer dimethyl silicone oil is controlled to be 330-370 mPa.s, and the viscosity of the component B can be adjusted to facilitate construction and application. Two coupling agents are compounded, so that the broad-spectrum adhesion of the two-component sealant to base materials such as anodized aluminum, float glass and the like is improved. The specific surface area of the carbon black is controlled to be 110-130m2The blackness of the component B and the solubility of the plasticizer can be balanced.
(2) When the component B is prepared, the polymethyltriethoxysilane, the plasticizer, the coupling agent I, the coupling agent II and the catalyst are weighed according to the proportion, are uniformly mixed under the protective atmosphere to avoid the water in the contact air from being hydrolyzed, and then the filler is added to uniformly mix with the liquid material under stirring to form a homogeneous phase.
(3) When the component B is prepared, the liquid material and the filler are uniformly mixed, and then stirred for 20-30 minutes in a vacuum state for dehydration.
(4) When the component B is prepared, the component B is treated by a bead mill, the viscosity of the component B is increased from 1-3 ten thousand cp to 5-12 ten thousand cp by bead milling, the sagging phenomenon is avoided, the construction and the application are convenient, meanwhile, the fineness of the component B can reach below 15 mu m, the glossiness is good, and the appearance after construction meets the requirements.
The invention adopts a horizontal bead mill, the coarsely mixed and uniform materials are conveyed into a closed grinding cylinder by a diaphragm pump, then the zirconium oxide grinding beads are pushed by a main machine to run at a high speed, so that the materials are pressurized and rotated at a high speed in a narrow grinding bead gap to generate the functions of mixing, dispersing, rolling and the like, thereby achieving the required fineness, and after grinding, the materials are output out of the grinding cylinder through a hard tungsten steel separation gap rotating at a high speed to carry out continuous circulating grinding. The traditional three-roller bead mill enables materials to achieve a grinding effect through mutual extrusion of the surfaces of the three horizontal rollers and friction at different speeds, is suitable for grinding small-batch materials, and is low in efficiency.
Detailed Description
The present invention will be described in further detail with reference to examples.
Example 1: a two-component silicone hollow glass sealant B component comprises the following components in parts by weight: 20g of polymethyl triethoxy silane, 30g of filler carbon black, 30g of plasticizer dimethyl silicone oil, 10g of coupling agent Igamma-aminopropyl triethoxy silane, 8g of coupling agent IIgamma- (2, 3-epoxypropoxy) propyl trimethoxy silane and 2g of catalyst dibutyltin dilaurate. Wherein the content of the polymethyl triethoxy silane is 85 wt%; the specific surface area of the carbon black is 125m2(ii)/g; the viscosity of the simethicone is 350 mPa.s. Polymethyl triethoxy silane is purchased from Zhejiang Quzhou Zhengbang organosilicon Co., Ltd., type No. 3 water repellent.
The preparation method comprises the following specific steps:
s1, weighing the polymethyltriethoxysilane, the plasticizer, the coupling agent I, the coupling agent II and the catalyst according to the proportion, adding the weighed materials into a planetary mixer, mixing for 5 minutes under the nitrogen protection atmosphere, controlling the temperature to be 40-45 ℃ in the stirring process, then adding the filler, and mixing for 5 minutes;
s2, stirring for 30 minutes under a vacuum state (the pressure is-0.095 MPa), then stopping the vacuum pump, and filling nitrogen to 0.02 MPa;
s3, transferring the material in the S2 to a bead mill for bead milling, wherein the pressure is 0.1MPa, the temperature is 30-40 ℃, and the time is 5 minutes, and the used milling beads are 2mm zirconium oxide during bead milling; the dosage ratio of the materials to the grinding beads is 3: 1; discharging after finishing the bead grinding, and controlling the temperature to be 10-20 ℃ during discharging. And sealing and packaging to obtain the component B of the double-component silicone hollow glass sealant.
Example 2: a two-component silicone hollow glass sealant B component comprises the following components in parts by weight: 25g of polymethyl triethoxy silane, 16g of filler carbon black, 35g of plasticizer dimethyl silicone oil, 15 g of coupling agent Igamma-aminopropyl triethoxy silane, 7g of coupling agent IIgamma- (2, 3-epoxypropoxy) propyl trimethoxy silane and 2g of catalyst dibutyltin dilaurate. Wherein the content of the polymethyl triethoxy silane is 95 percent; the specific surface area of the carbon black is 110m2(ii)/g; the viscosity of the dimethylsilicone fluid was 370 mPa.s.
The preparation method comprises the following specific steps:
s1, weighing the polymethyltriethoxysilane, the plasticizer, the coupling agent I, the coupling agent II and the catalyst according to a ratio, adding the weighed materials into a planetary mixer, mixing the materials for 10 minutes under the nitrogen protection atmosphere, controlling the temperature to be 50-60 ℃ in the stirring process, then adding the filler, and mixing the materials for 10 minutes;
s2, stirring for 25 minutes under a vacuum state (the pressure is-0.085 MPa), then stopping the vacuum pump, and filling nitrogen to 0.01 MPa;
s3, transferring the material in the S2 to a bead mill for bead milling, wherein the pressure is 0.2MPa, the temperature is 40-50 ℃, the time is 10 minutes, and the bead milling size is 3mm and the material is zirconium oxide during bead milling; the dosage ratio of the materials to the grinding beads is 3: 1; discharging after finishing the bead grinding, and controlling the temperature to be 20-30 ℃ during discharging. And sealing and packaging to obtain the component B of the double-component silicone hollow glass sealant.
Example 3:
a two-component silicone hollow glass sealant B component comprises the following components in parts by weight: 20g of polymethyl triethoxy silane, 10g of filler carbon black, 50g of plasticizer dimethyl silicone oil, 12 g of coupling agent Igamma-aminopropyl triethoxy silane, 5g of coupling agent IIgamma- (2, 3-epoxypropoxy) propyl trimethoxy silane and 3g of catalyst dibutyltin dilaurate. Wherein the content of the polymethyl triethoxy silane is 90 percent; the specific surface area of the carbon black is 130m2(ii)/g; the viscosity of the dimethicone was 330 mPa.s。
The preparation method comprises the following specific steps:
s1, weighing the polymethyltriethoxysilane, the plasticizer, the coupling agent I, the coupling agent II and the catalyst according to a ratio, adding the weighed materials into a planetary mixer, mixing for 7 minutes under the nitrogen protection atmosphere, controlling the temperature to be 50-60 ℃ in the stirring process, then adding the filler, and mixing for 7 minutes;
s2, stirring for 20 minutes under a vacuum state (the pressure is-0.088 MPa), then stopping the vacuum pump, and filling nitrogen to 0.01 MPa;
s3, transferring the material in the S2 to a bead mill for bead milling, wherein the pressure is 0.3MPa, the temperature is 35-45 ℃, the time is 7 minutes, and the bead milling size is 2mm and the material is zirconium oxide during bead milling; the dosage ratio of the materials to the grinding beads is 3: 1; discharging after finishing the bead grinding, and controlling the temperature to be 20-30 ℃ during discharging. And sealing and packaging to obtain the component B of the double-component silicone hollow glass sealant.
Example 4:
a two-component silicone hollow glass sealant B component comprises the following components in parts by weight: 35g of polymethyl triethoxy silane, 10g of filler carbon black, 34g of plasticizer dimethyl silicone oil, 15 g of coupling agent Igamma-aminopropyl triethoxy silane, 5g of coupling agent IIgamma- (2, 3-epoxypropoxy) propyl trimethoxy silane and 1g of catalyst dibutyltin dilaurate. Wherein the content of the polymethyl triethoxy silane is 92 percent; the specific surface area of the carbon black is 118m2(ii)/g; the viscosity of the simethicone is 340 mPa.s.
The preparation method comprises the following specific steps:
s1, weighing the polymethyltriethoxysilane, the plasticizer, the coupling agent I, the coupling agent II and the catalyst according to a ratio, adding the weighed materials into a planetary mixer, mixing for 9 minutes under the nitrogen protection atmosphere, controlling the temperature to be 50-60 ℃ in the stirring process, then adding the filler, and mixing for 9 minutes;
s2, stirring for 28 minutes under a vacuum state (the pressure is-0.092 MPa), then stopping the vacuum pump, and filling nitrogen to 0.15 MPa;
s3, transferring the material in the S2 to a bead mill for bead milling, wherein the pressure is 0.2MPa, the temperature is 40-50 ℃, the time is 9 minutes, and the bead milling size is 3mm and the material is zirconium oxide during bead milling; the dosage ratio of the materials to the grinding beads is 3: 1; discharging after finishing the bead grinding, and controlling the temperature to be 20-30 ℃ during discharging. And sealing and packaging to obtain the component B of the double-component silicone hollow glass sealant.
Example 5:
a two-component silicone hollow glass sealant B component has the same formula and dosage as in example 1.
The preparation method comprises the following specific steps:
s1, weighing the polymethyltriethoxysilane, the plasticizer, the coupling agent I, the coupling agent II and the catalyst according to the proportion, adding the weighed materials into a planetary mixer, mixing for 5 minutes under the nitrogen protection atmosphere, controlling the temperature to be 40-45 ℃ in the stirring process, then adding the filler, and mixing for 5 minutes;
s2, stirring for 30 minutes under a vacuum state (the pressure is-0.095 MPa), then stopping the vacuum pump, and filling nitrogen to 0.02 MPa;
s3, transferring the material in the S2 to a three-roll bead mill for bead milling, wherein the diameter of a roller is 65mm, the length of the roller is 125mm, the rotating speed of the roller is 32r/min, the temperature is 30-40 ℃, the time is 10 minutes, discharging is carried out after the bead milling is finished, and the temperature is controlled to be 10-20 ℃ during discharging. And sealing and packaging to obtain the component B of the double-component silicone hollow glass sealant.
By comparing example 1 with example 5, the formula is the same, and the time used in example 1 is 1/2 of example 5, and the efficiency is obviously higher.
Example 6:
a two-component silicone hollow glass sealant B component, the formula of which is general to example 2.
The preparation method comprises the following specific steps:
s1, weighing the polymethyltriethoxysilane, the plasticizer, the coupling agent I, the coupling agent II and the catalyst according to a ratio, adding the weighed materials into a planetary mixer, mixing the materials for 10 minutes under the nitrogen protection atmosphere, controlling the temperature to be 50-60 ℃ in the stirring process, then adding the filler, and mixing the materials for 10 minutes;
s2, transferring the material in the S1 to a bead mill for bead milling, wherein the pressure is 0.2MPa, the temperature is 40-50 ℃, the time is 10 minutes, and the bead milling size is 3mm and the material is zirconium oxide during bead milling; the dosage ratio of the materials to the grinding beads is 3: 1; discharging after finishing the bead grinding, and controlling the temperature to be 20-30 ℃ during discharging. And sealing and packaging to obtain the component B of the double-component silicone hollow glass sealant.
By comparing the example 2 with the example 6, the formula is the same, the stirring in the vacuum environment is not performed in the example 6, the viscosity detection result of the component B obtained in the example 2 is 6.5 ten thousand cp, the construction requirement is met, and the viscosity detection result of the component B obtained in the example 6 is 4.2 ten thousand cp, and the viscosity is lower than 5 ten thousand cp.
Example 7:
a two-component silicone hollow glass sealant B component was formulated as in example 3.
The preparation method comprises the following specific steps:
s1, weighing the polymethyltriethoxysilane, the plasticizer, the coupling agent I, the coupling agent II and the catalyst according to a ratio, adding the weighed materials into a planetary mixer, mixing for 7 minutes under the nitrogen protection atmosphere, controlling the temperature to be 50-60 ℃ in the stirring process, then adding the filler, and mixing for 7 minutes;
s2, stirring for 20 minutes under a vacuum state (the pressure is-0.088 MPa), then stopping the vacuum pump, and filling nitrogen to 0.01 MPa;
s3, sealing and packaging the materials in the S2 to obtain the component B of the bi-component silicone hollow glass sealant.
By comparing the example 3 with the example 7, the formula is the same, the bead milling treatment is not carried out in the preparation process of the example 7, the viscosity detection result of the component B obtained in the example 3 is 6.1 ten thousands cp, the construction requirement is met, and the viscosity detection result of the component B obtained in the example 7 is 2.8 ten thousands cp, and the viscosity is lower than 5 ten thousands cp.
Example 8:
a two-component silicone hollow glass sealant B component was formulated as in example 4.
The preparation method comprises the following specific steps:
s1, weighing the polymethyltriethoxysilane, the plasticizer, the coupling agent I, the coupling agent II and the catalyst according to a ratio, adding the weighed materials into a planetary mixer, mixing for 9 minutes under the nitrogen protection atmosphere, controlling the temperature to be 50-60 ℃ in the stirring process, then adding the filler, and mixing for 9 minutes;
s2, stirring for 28 minutes under a vacuum state (the pressure is-0.092 MPa), then stopping the vacuum pump, and filling nitrogen to 0.15 MPa;
s3, transferring the material in the S2 to a bead mill for bead milling, wherein the pressure is 0.2MPa, the temperature is 40-50 ℃, the time is 9 minutes, and the bead milling size is 3mm and the material is zirconium oxide during bead milling; the dosage ratio of the materials to the grinding beads is 5: 1; discharging after finishing the bead grinding, and controlling the temperature to be 20-30 ℃ during discharging. And sealing and packaging to obtain the component B of the double-component silicone hollow glass sealant.
By comparing the example 4 with the example 8, the formula is the same, the dosage ratio of the material and the grinding beads in the example 8 is 5:1, the dosage ratio of the material and the grinding beads in the example 4 is 3:1, the viscosity detection result of the component B obtained in the example 4 is 6.8 ten-thousand-cp, the construction requirement is met, the viscosity detection result of the component B obtained in the example 8 is 4.5 ten-thousand-cp, and the viscosity is lower than 5 ten-thousand-cp.
The above-described embodiments are merely preferred embodiments of the present invention, and should not be construed as limiting the present invention, and features in the embodiments and examples in the present application may be arbitrarily combined with each other without conflict. The protection scope of the present invention is defined by the claims, and includes equivalents of technical features of the claims. I.e., equivalent alterations and modifications within the scope hereof, are also intended to be within the scope of the invention.
Claims (10)
1. The component B of the two-component silicone hollow glass sealant is characterized by comprising the following components in parts by weight: 20-40 parts of polymethyl triethoxy silane, 10-30 parts of filler, 30-50 parts of plasticizer, 10-15 parts of coupling agent I, 5-10 parts of coupling agent II and 1-3 parts of catalyst.
2. The two-component silicone hollow glass sealant B component of claim 1, wherein: the content of the polymethyl triethoxy silane is 85-95%.
3. The two-component silicone hollow glass sealant B component of claim 1, wherein: the filler is carbon black, and the specific surface area of the carbon black is 110-130m2/g。
4. The two-component silicone hollow glass sealant B component of claim 1, wherein: the plasticizer is dimethyl silicone oil, and the viscosity is 330-370 mPa.s.
5. The two-component silicone hollow glass sealant B component of claim 1, wherein: the coupling agent I is gamma-aminopropyl triethoxysilane; the coupling agent II is gamma- (2, 3-epoxypropoxy) propyl trimethoxy silane; the catalyst was dibutyltin dilaurate.
6. The method for preparing the B component of the two-component silicone hollow glass sealant as claimed in any one of claims 1 to 5, which is characterized by comprising the following steps:
s1, weighing the polymethyltriethoxysilane, the plasticizer, the coupling agent I, the coupling agent II and the catalyst according to the proportion, uniformly mixing under a protective atmosphere, adding the filler, and uniformly mixing;
s2, stirring for 20-30 minutes in a vacuum state, stopping the vacuum pump, and filling nitrogen to 0.01-0.02 MPa;
and S3, transferring the material in the S2 to a bead mill for bead milling under the pressure of 0.1-0.3MPa and at the temperature of 30-50 ℃ for 5-10 minutes, discharging after the bead milling is finished, and sealing and packaging to obtain the component B of the bi-component silicone hollow glass sealant.
7. The method according to claim 6, wherein: and in the S1, the mixing equipment is a planetary mixer, the temperature is controlled to be 40-60 ℃ in the stirring process, the mixture is stirred for 5-10 minutes in a nitrogen environment, and the mixture is stirred for 5-10 minutes after the filler is added.
8. The method according to claim 6, wherein: the pressure in S2 is-0.085 to-0.095 MPa.
9. The method according to claim 6, wherein: in the S3 process of bead grinding, the used grinding beads have the diameter of 2-3mm and are made of zirconia.
10. The method of claim 8, wherein: and controlling the temperature to be 10-30 ℃ during discharging in S3.
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