CN107880841B - Anti-fog automobile lamp silicone sealant and preparation method thereof - Google Patents
Anti-fog automobile lamp silicone sealant and preparation method thereof Download PDFInfo
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- CN107880841B CN107880841B CN201711354610.1A CN201711354610A CN107880841B CN 107880841 B CN107880841 B CN 107880841B CN 201711354610 A CN201711354610 A CN 201711354610A CN 107880841 B CN107880841 B CN 107880841B
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- 239000004590 silicone sealant Substances 0.000 title claims abstract description 28
- 238000002360 preparation method Methods 0.000 title claims abstract description 14
- 229920002379 silicone rubber Polymers 0.000 claims abstract description 28
- 239000003431 cross linking reagent Substances 0.000 claims abstract description 19
- 239000000843 powder Substances 0.000 claims abstract description 17
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 claims abstract description 14
- 229910052791 calcium Inorganic materials 0.000 claims abstract description 14
- 239000011575 calcium Substances 0.000 claims abstract description 14
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 13
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 13
- 229910052799 carbon Inorganic materials 0.000 claims abstract description 13
- 229910021485 fumed silica Inorganic materials 0.000 claims abstract description 13
- 238000000034 method Methods 0.000 claims abstract description 13
- 239000002002 slurry Substances 0.000 claims abstract description 13
- 239000003054 catalyst Substances 0.000 claims abstract description 12
- 230000008569 process Effects 0.000 claims abstract description 9
- 239000007822 coupling agent Substances 0.000 claims abstract description 7
- 239000000463 material Substances 0.000 claims description 18
- 238000003756 stirring Methods 0.000 claims description 14
- 238000004806 packaging method and process Methods 0.000 claims description 8
- 238000004898 kneading Methods 0.000 claims description 7
- 238000001816 cooling Methods 0.000 claims description 5
- 239000006185 dispersion Substances 0.000 claims description 5
- 238000006116 polymerization reaction Methods 0.000 claims description 5
- -1 alkyl trimethoxy silane Chemical compound 0.000 claims description 4
- 239000002245 particle Substances 0.000 claims description 4
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims description 2
- 239000010941 cobalt Substances 0.000 claims description 2
- 229910017052 cobalt Inorganic materials 0.000 claims description 2
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 claims description 2
- 239000000945 filler Substances 0.000 claims description 2
- 230000003301 hydrolyzing effect Effects 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 claims description 2
- 238000002156 mixing Methods 0.000 claims description 2
- 229920000642 polymer Polymers 0.000 claims description 2
- 230000000379 polymerizing effect Effects 0.000 claims description 2
- 229910000077 silane Inorganic materials 0.000 claims description 2
- 239000012974 tin catalyst Substances 0.000 claims description 2
- 239000010936 titanium Substances 0.000 claims description 2
- 229910052719 titanium Inorganic materials 0.000 claims description 2
- 239000000565 sealant Substances 0.000 abstract description 21
- 239000011248 coating agent Substances 0.000 abstract description 7
- 238000000576 coating method Methods 0.000 abstract description 7
- 239000000126 substance Substances 0.000 abstract description 4
- 230000000694 effects Effects 0.000 abstract description 3
- 239000004831 Hot glue Substances 0.000 description 25
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 14
- 125000000484 butyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 description 13
- 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 description 11
- 238000012360 testing method Methods 0.000 description 11
- 239000004945 silicone rubber Substances 0.000 description 9
- 239000000203 mixture Substances 0.000 description 5
- OECBPUHKHTYFET-UHFFFAOYSA-J tris(decanoyloxy)stannyl decanoate Chemical compound [Sn+4].CCCCCCCCCC([O-])=O.CCCCCCCCCC([O-])=O.CCCCCCCCCC([O-])=O.CCCCCCCCCC([O-])=O OECBPUHKHTYFET-UHFFFAOYSA-J 0.000 description 5
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 4
- 230000008859 change Effects 0.000 description 4
- 229910052710 silicon Inorganic materials 0.000 description 4
- 239000010703 silicon Substances 0.000 description 4
- YYRMJZQKEFZXMX-UHFFFAOYSA-N calcium;phosphoric acid Chemical compound [Ca+2].OP(O)(O)=O.OP(O)(O)=O YYRMJZQKEFZXMX-UHFFFAOYSA-N 0.000 description 3
- 238000009833 condensation Methods 0.000 description 3
- 230000005494 condensation Effects 0.000 description 3
- KPUWHANPEXNPJT-UHFFFAOYSA-N disiloxane Chemical class [SiH3]O[SiH3] KPUWHANPEXNPJT-UHFFFAOYSA-N 0.000 description 3
- 230000005855 radiation Effects 0.000 description 3
- 238000007789 sealing Methods 0.000 description 3
- 230000035939 shock Effects 0.000 description 3
- 238000005507 spraying Methods 0.000 description 3
- 239000002426 superphosphate Substances 0.000 description 3
- 230000007547 defect Effects 0.000 description 2
- 238000013461 design Methods 0.000 description 2
- 238000009826 distribution Methods 0.000 description 2
- 239000012943 hotmelt Substances 0.000 description 2
- MTEZSDOQASFMDI-UHFFFAOYSA-N 1-trimethoxysilylpropan-1-ol Chemical compound CCC(O)[Si](OC)(OC)OC MTEZSDOQASFMDI-UHFFFAOYSA-N 0.000 description 1
- 230000006750 UV protection Effects 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 239000000853 adhesive Substances 0.000 description 1
- 230000001070 adhesive effect Effects 0.000 description 1
- 230000032683 aging Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 238000005336 cracking Methods 0.000 description 1
- GHVNFZFCNZKVNT-UHFFFAOYSA-N decanoic acid Chemical compound CCCCCCCCCC(O)=O GHVNFZFCNZKVNT-UHFFFAOYSA-N 0.000 description 1
- 230000001066 destructive effect Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000011049 filling Methods 0.000 description 1
- 238000009472 formulation Methods 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 238000007689 inspection Methods 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000003973 paint Substances 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 230000008054 signal transmission Effects 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
- 238000005406 washing Methods 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
- C09J183/06—Polysiloxanes containing silicon bound to oxygen-containing groups
-
- 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
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/02—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group
- C08L2205/025—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group containing two or more polymers of the same hierarchy C08L, and differing only in parameters such as density, comonomer content, molecular weight, structure
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Sealing Material Composition (AREA)
Abstract
The invention discloses an anti-fog automobile lamp silicone sealant which comprises the following components in parts by weight: 10-30 parts of 80000-5000000mPa & s alkoxy-terminated 107 silicon rubber, 10-40 parts of 1000-80000mPa & s alkoxy-terminated 107 silicon rubber, 30-50 parts of calcium powder, 1-10 parts of fumed silica, 1-10 parts of carbon slurry, 1-5 parts of macromolecular cross-linking agent, 1-5 parts of coupling agent and 0.1-5 parts of catalyst. The invention also provides a preparation method of the anti-fog automobile lamp silicone sealant. According to the antifogging automobile lamp silicone sealant, the alkoxy-terminated 107 silicon rubber and the macromolecular cross-linking agent are used for replacing the traditional 107 silicon rubber and the single-molecular cross-linking agent, so that substances which have damage effects on an automobile lamp antifogging coating are not generated in the curing and using processes. The invention is dealcoholized room temperature vulcanized organosilicon sealant which is environment-friendly.
Description
Technical Field
The invention relates to a sealant and a preparation method thereof, in particular to an anti-fog automobile lamp silicone sealant and a preparation method thereof, and belongs to the technical field of anti-fog automobile lamp sealing.
Background
With the continuous progress of the automobile industry, people have higher and higher requirements on the running reliability of automobiles. The automobile lamp is used as an automobile lighting and signal transmission tool and has a vital influence on the automobile driving safety. The main reason that quality problems appear in present car light is that the car light that sealed inefficacy leads to intakes and hazes, not only influences the life and the outward appearance of car light, makes the illuminating effect descend by a wide margin moreover, brings the potential safety hazard for the personnel of driving in. The automobile lamp after-sale claim caused by the fogging problem is high every year, and the automobile lamp after-sale claim always troubles a plurality of automobile factories and automobile lamp manufacturers. In daily use, the phenomenon of fogging of the lamps is very common, and the lamps generate fogging to different degrees in rainy seasons or after car washing. With the improvement of safety awareness of people, it has become necessary to solve the problems of water inflow and fogging of the car lights.
The fog of general car light needs to satisfy 3 conditions: (1) a condensation core exists inside the car lamp; (2) the temperature difference exists in different areas inside the car lamp; (3) a sufficient concentration of water vapor is present inside the vehicle lamp. Because the sealed bad steam that leads to in the environment of car light gets into the lamp body in a large number inside, when the inside temperature of car light was less than this part steam's critical saturation temperature, will form the drop of water and adsorb in the lamp intracavity to accumulate gradually and form ponding. When the car light is turned on, the ambient temperature around the light source will rise sharply, the accumulated water in the lamp will begin to evaporate into water vapor under the action of heat radiation and convection heat transfer, and the water vapor will diffuse to various areas of the car light. In order to meet the requirements of modeling and appearance, the aspect ratio and depth ratio of the car lamp are larger and larger, the shape is longer and narrower, and the temperature distribution of each area inside the car lamp is uneven, so when water vapor is diffused from an area with higher humidity and temperature to an area with lower temperature, water drops can be condensed to be attached to the surface of a lampshade, light rays are irradiated on the water drops to generate diffuse reflection, and the fogging phenomenon is caused.
Vehicle lamp manufacturers now generally reduce vehicle lamp fogging by the following 6 methods: (1) controlling the internal humidity of the vehicle lamp, and keeping the humidity of vehicle lamp parts and the humidity of the production environment in a conventional state; (2) the structure design eliminates the areas of the radiation and convection dead angles of the car lamp; (3) an antifogging coating spraying process is added on the inner surface of the lampshade to convert water vapor from drop condensation into film condensation; (4) properly adjusting the number of air holes of the car lamp, changing the position and the size, and promoting the timely convection of water vapor as much as possible; (5) according to the design principle, the reflector of the car lamp is adjusted in shape and bulb position, and the distribution of the radiation field is changed; (6) the sealing performance of the automobile lamp is enhanced, and the water is effectively reduced. Emerging material technology brings more fogging solutions to us, and spraying an antifogging coating is the simplest and most effective method.
The most common in the current vehicle lamp sealant industry are traditional silicone rubber, butyl hot melt adhesive and PUR hot melt adhesive. The traditional organosilicon sealant has good weather resistance and ultraviolet resistance, and good shock resistance and cold and hot shock resistance, but substances generated in the curing process can seriously damage the antifogging coating. The sealing performance and the shock resistance of the butyl hot melt adhesive and the PUR hot melt adhesive are good, and the antifogging coating is not damaged. But the weather resistance and the aging resistance of the hot melt adhesive are not as good as those of the organic silicon sealant, and the requirements of the hot melt adhesive on packaging and construction equipment are much higher than those of the traditional organic silicon sealant.
Disclosure of Invention
The invention overcomes the defects of the prior art and provides an antifogging automobile lamp silicone sealant and a preparation method thereof. The alkoxy-terminated 107 silicon rubber and the macromolecular cross-linking agent are used for replacing the traditional 107 silicon rubber and the monomolecular cross-linking agent, so that the novel antifogging silicone sealant for the automobile lamp is obtained. The sealant not only keeps the excellent elasticity, cracking resistance and impact resistance of the traditional organosilicon sealant, but also does not generate substances which have destructive effect on the car lamp antifogging coating in the curing and using processes, breaks through the application defect of the traditional organosilicon sealant, and has wide prospect in the field of car lamp sealants.
In order to solve the technical problems, the invention adopts the following technical scheme:
an anti-fog automobile lamp silicone sealant comprises the following components in parts by weight:
10-30 parts of 80000-5000000mPa & s alkoxy-terminated 107 silicon rubber, 10-40 parts of 1000-80000mPa & s alkoxy-terminated 107 silicon rubber, 30-50 parts of calcium powder, 1-10 parts of fumed silica, 1-10 parts of carbon slurry, 1-5 parts of macromolecular cross-linking agent, 1-5 parts of coupling agent and 0.1-5 parts of catalyst.
The further technical scheme is as follows:
the alkoxy-terminated 107 silicone rubber refers to a polymer obtained after the 107 silicone rubber is terminated by alkyl trimethoxy silane.
The further technical scheme is as follows:
the calcium powder is heavy calcium powder or/and light calcium powder used as filler, and the particle size is 0.01-100 microns.
The further technical scheme is as follows:
the fumed silica has a specific surface area of 50m2/g-400m2/g。
The further technical scheme is as follows:
the particle size of the carbon slurry is 1-1000 nm.
The further technical scheme is as follows:
the macromolecular cross-linking agent is an oligomer with the polymerization degree of 2-50 formed by hydrolyzing and polymerizing alkoxy silane.
The further technical scheme is as follows:
the coupling agent is one or more of KH470, KH530, KH540, KH550, KH560, KH570, KH580, KH590, KH602, KH791, KH792, KH901 and KH 910.
The further technical scheme is as follows:
the catalyst is one or more of an organic tin catalyst, an organic titanium catalyst and an organic cobalt catalyst.
The invention also provides a preparation method of the anti-fog automobile lamp silicone sealant.
The preparation method of the anti-fog automobile lamp silicone sealant comprises the following steps:
adding alkoxy-terminated 107 silicon rubber and calcium powder with different viscosities, fumed silica and carbon slurry into a kneader, kneading at the temperature of 130-150 ℃ and the pressure of-0.09-0.095 MPa to prepare a base material, cooling to normal temperature, and storing in a sealed manner for later use;
through the first step, the moisture in the material can be removed, and the preparation is made for subsequent treatment.
Step two, adding the base material into a high-speed dispersion machine, evacuating and defoaming, adding the macromolecular cross-linking agent, and stirring in a vacuum state, wherein the vacuum is less than-0.08 MPa in the process;
step three, adding a coupling agent, keeping the air and stirring the mixture until the vacuum is less than-0.08 MPa;
and step four, adding a catalyst, evacuating, dispersing at a high speed for 30 minutes, and packaging to obtain the product.
The further technical scheme is as follows:
and in the second step and the third step, after the mixture is kept empty and stirred, if the vacuum is more than-0.08 MPa, the mixture is timely vacuumized to maintain the vacuum to be less than-0.08 MPa. And finally, filling the sealant can be finished after vacuum defoaming treatment.
The further technical scheme is as follows:
and the relative humidity of the mixing environment in the first step, the second step and the fourth step is lower than 70%.
The lower relative humidity is to ensure that the catalyst is not deactivated and the reaction efficiency is improved.
The further technical scheme is as follows:
kneading for 4 hours in the first step to prepare a base material;
in the second step, the vacuumizing and defoaming time is 10 minutes, and the air-holding and stirring time is 20 minutes;
the air-holding stirring time in the third step is 20 minutes.
Compared with the prior art, one of the beneficial effects of the embodiment of the invention is as follows:
according to the antifogging automobile lamp silicone sealant, the alkoxy-terminated 107 silicon rubber and the macromolecular cross-linking agent are used for replacing the traditional 107 silicon rubber and the single-molecular cross-linking agent, so that substances which have damage effects on an automobile lamp antifogging coating are not generated in the curing and using processes.
The invention is dealcoholized room temperature vulcanized organosilicon sealant which is environment-friendly.
Most of the raw materials adopted by the invention are easy to obtain, the preparation process is simple, and the method is suitable for large-scale industrial production and application.
Detailed Description
All of the features disclosed in this specification, or all of the steps in any method or process so disclosed, may be combined in any combination, except combinations of features and/or steps that are mutually exclusive.
Any feature disclosed in this specification (including any accompanying claims, abstract) may be replaced by alternative features serving equivalent or similar purposes, unless expressly stated otherwise. That is, unless expressly stated otherwise, each feature is only an example of a generic series of equivalent or similar features.
The following describes in detail a specific embodiment of the present invention with reference to examples.
Example 1
According to one embodiment of the invention, the embodiment discloses an antifogging automobile lamp silicone sealant, which is prepared by the following formula: 20kg of 80000 mPas alkoxy-terminated 107 silicone rubber, 20kg of 20000 mPas alkoxy-terminated 107 silicone rubber, 40kg of 20-micron heavy calcium powder and 50m of22kg of fumed silica, 0.2kg of 50-nanometer carbon slurry, 0.3kg of polymethyl trimethoxy siloxane macromolecular cross-linking agent with the polymerization degree of 2-50, 0.3kg of gamma-methacryloxypropyl trimethoxy silane (KH-570) and 0.05kg of tin decanoate.
Further, the preparation method of the anti-fog automobile lamp silicone sealant is realized by the following steps:
adding two types of alkoxy-terminated 107 silicon rubber with different viscosities, triple superphosphate powder, fumed silica and carbon slurry into a kneader, kneading for 4 hours at the temperature of 130-150 ℃ and the pressure of-0.09-0.095 MPa to prepare a base material, cooling to normal temperature, and storing in a sealed manner for later use;
and (2) adding the base material into a high-speed dispersion machine, evacuating and defoaming for 10 minutes, removing air mixed in the base material as much as possible, adding the macromolecular cross-linking agent, and stirring for 20 minutes in an air-preserved manner, wherein the vacuum requirement is less than-0.08 MPa. If the vacuum is more than-0.08 MPa, vacuumizing in time to maintain the vacuum to be less than-0.08 MPa.
And (3) adding gamma-methacryloxypropyltrimethoxysilane (KH-570), and stirring for 20 minutes in vacuum with the vacuum being less than-0.08 MPa. If the vacuum is more than-0.08 MPa, timely vacuumizing to maintain the vacuum to be less than-0.08 MPa
And (4) adding tin decanoate, evacuating, dispersing at high speed for 30 minutes, and packaging to obtain the product.
Example 2
In accordance with a second embodiment of the present invention, this example discloses an anti-fog automotive lamp silicone sealant, which is formulated as follows: 15kg of 5000000 mPas alkoxyl-terminated 107 silicone rubber, 20kg of 1000 mPas alkoxyl-terminated 107 silicone rubber, 45kg of 20 micron heavy calcium powder and 50m of the mixture22kg of fumed silica, 0.2kg of 50-nanometer carbon slurry, 0.3kg of polymethyl trimethoxy siloxane macromolecular cross-linking agent with the polymerization degree of 2-50 and gamma-methacryloyl0.3kg of oxypropyltrimethoxysilane (KH-570) and 0.05kg of stannic decanoate.
The preparation method of the anti-fog automobile lamp silicone sealant is realized by the following steps:
adding two types of alkoxy-terminated 107 silicon rubber with different viscosities, triple superphosphate powder, fumed silica and carbon slurry into a kneader, kneading for 4 hours at the temperature of 130-150 ℃ and the pressure of-0.09-0.095 MPa to prepare a base material, cooling to normal temperature, and storing in a sealed manner for later use;
and (2) adding the base material into a high-speed dispersion machine, evacuating and defoaming for 10 minutes, removing air mixed in the base material as much as possible, adding the macromolecular cross-linking agent, and stirring for 20 minutes in an air-preserved manner, wherein the vacuum requirement is less than-0.08 MPa. If the vacuum is more than-0.08 MPa, vacuumizing in time to maintain the vacuum to be less than-0.08 MPa.
And (3) adding gamma-methacryloxypropyltrimethoxysilane (KH-570), and stirring for 20 minutes in vacuum with the vacuum being less than-0.08 MPa. If the vacuum is more than-0.08 MPa, timely vacuumizing to maintain the vacuum to be less than-0.08 MPa
And (4) adding tin decanoate, evacuating, dispersing at high speed for 30 minutes, and packaging to obtain the product.
Example 3
According to a third embodiment of the invention, the present example discloses an anti-fog automotive lamp silicone sealant, which has the following formula: 15kg of alkoxy-terminated 107 silicone rubber of 200000 mPas, 15kg of alkoxy-terminated 107 silicone rubber of 80000 mPas, 50kg of 20-micron heavy calcium powder and 50m22kg of fumed silica, 0.2kg of 50-nanometer carbon slurry, 0.3kg of polymethyl trimethoxy siloxane macromolecular cross-linking agent with the polymerization degree of 2-50, 0.3kg of gamma-methacryloxypropyl trimethoxy silane (KH-570) and 0.05kg of tin decanoate.
The preparation method of the anti-fog automobile lamp silicone sealant is realized by the following steps:
adding two types of alkoxy-terminated 107 silicon rubber with different viscosities, triple superphosphate powder, fumed silica and carbon slurry into a kneader, kneading for 4 hours at the temperature of 130-150 ℃ and the pressure of-0.09-0.095 MPa to prepare a base material, cooling to normal temperature, and storing in a sealed manner for later use;
and (2) adding the base material into a high-speed dispersion machine, evacuating and defoaming for 10 minutes, removing air mixed in the base material as much as possible, adding the macromolecular cross-linking agent, and stirring for 20 minutes in an air-preserved manner, wherein the vacuum requirement is less than-0.08 MPa. If the vacuum is more than-0.08 MPa, vacuumizing in time to maintain the vacuum to be less than-0.08 MPa.
And (3) adding gamma-methacryloxypropyltrimethoxysilane (KH-570), and stirring for 20 minutes in vacuum with the vacuum being less than-0.08 MPa. If the vacuum is more than-0.08 MPa, timely vacuumizing to maintain the vacuum to be less than-0.08 MPa
And (4) adding tin decanoate, evacuating, dispersing at high speed for 30 minutes, and packaging to obtain the product.
Examples 2 and 3 the formulation and process were exactly the same as in example 1, except that the solid-to-liquid ratio was different from that in example 1.
The adhesives prepared in example 1, example 2 and example 3 were compared with commercially available butyl hot melt adhesives and PUR hot melt adhesives and used for bonding PC and PP (plasma treated) sample sheets together, and the results of testing the bonding performance of the silicone sealant are shown in Table 1 with reference to GB/T7124-2008.
The prepared sealant is used for packaging the car lamp by comparing a commercially available butyl hot melt adhesive and a PUR hot melt adhesive, the car lamp is turned on after being maintained for one week, the fogging condition of the car lamp is tested in a spraying environment, and the test result is shown in Table 2.
The prepared sealant is used for packaging automobile lamps compared with commercially available butyl hot melt adhesive and PUR hot melt adhesive, the automobile lamps are maintained for 24 hours and then inflated to 5000Pa (pressurization time is 15s, holding time is 10s, and inspection time is 8 s), the attenuation value of the pressure is observed, and the automobile lamps are qualified when the attenuation value is less than 50 Pa. The test results are shown in table 3.
The prepared sealant is compared with commercially available butyl hot melt adhesives and PUR hot melt adhesives to prepare a dumbbell test piece, the tensile strength and elongation at break of the three sealants are compared after the three sealants are subjected to water ultraviolet treatment for one week, the weather resistance of the three sealants is verified, and the mechanical test is referred to GB/T528-. The test results are shown in table 4.
TABLE 1
As shown in table 1, the three examples showed significantly better adhesion to the substrate than the butyl hot melt, which is substantially comparable to the shear strength of conventional silicone sealants and PUR hot melt.
TABLE 2
As shown in table 2: in the automobile lamp fogging test, the experimental results of the three embodiments are superior to those of the traditional organosilicon sealant, and are equivalent to those of butyl hot melt adhesive and PUR hot melt adhesive.
TABLE 3
As shown in table 3: compared with the three comparative examples, the three examples have the pressure attenuation smaller than 50Pa and meet the air tightness requirement of the vehicle lamp.
TABLE 4
As shown in table 4: after the dumbbell test piece is subjected to water ultraviolet treatment for one week, the tensile strength change rate and the elongation change rate of the dumbbell test piece in the three examples are far smaller than those of butyl hot melt adhesive and PUR hot melt adhesive, and the weather resistance of the dumbbell test piece in the three examples is better than that of the butyl hot melt adhesive and the PUR hot melt adhesive. The tensile strength change rate and the elongation change rate of the three examples are basically equivalent to those of the traditional organic silicon, and the weather resistance of the three examples is basically equivalent to that of the traditional organic silicon.
Through four experimental results, we can know that: the bonding performance of the embodiment of the invention to the base material of the vehicle lamp is superior to that of butyl hot melt adhesive; the paint is superior to the traditional organosilicon sealant in the fogging experiment of the car lamp; is superior to butyl hot melt adhesive and PUR hot melt adhesive in weather resistance test. In conclusion, the embodiments of the invention are superior to commercially available butyl hot melt adhesives, PUR hot melt adhesives and traditional organosilicon sealants in comprehensive performance.
Although the present invention has been described herein with reference to the illustrated embodiments thereof, which are intended to be preferred embodiments of the present invention, it is to be understood that the invention is not limited thereto, and that numerous other modifications and embodiments can be devised by those skilled in the art that will fall within the spirit and scope of the principles of this disclosure.
Claims (8)
1. An antifog automobile lamp silicone sealant is characterized by comprising the following components in parts by weight: 10-30 parts of 80000-5000000mPa & s alkoxy-terminated 107 silicon rubber, 10-40 parts of 1000-80000mPa & s alkoxy-terminated 107 silicon rubber, 30-50 parts of calcium powder, 1-10 parts of fumed silica, 1-10 parts of carbon slurry, 0.3 part of macromolecular cross-linking agent, 0.3 part of coupling agent and 0.05 part of catalyst;
the alkoxy-terminated 107 silicon rubber is a polymer obtained by terminating 107 silicon rubber with alkyl trimethoxy silane;
the macromolecular cross-linking agent is an oligomer with the polymerization degree of 2-50 formed by hydrolyzing and polymerizing alkoxy silane.
2. The anti-fog automotive lamp silicone sealant according to claim 1, characterized in that:
the calcium powder is heavy calcium powder or/and light calcium powder used as filler, and the particle size is 0.01-100 microns.
3. The anti-fog automotive lamp silicone sealant according to claim 1, characterized in that:
the fumed silica has a specific surface area of 50m2/g-400m2/g。
4. The anti-fog automotive lamp silicone sealant according to claim 1, characterized in that:
the particle size of the carbon slurry is 1-1000 nm.
5. The anti-fog automotive lamp silicone sealant according to claim 1, characterized in that:
the coupling agent is one or more of KH470, KH530, KH540, KH550, KH560, KH570, KH580, KH590, KH602, KH791, KH792, KH901 and KH 910.
6. The anti-fog automotive lamp silicone sealant according to claim 1, characterized in that:
the catalyst is one or more of an organic tin catalyst, an organic titanium catalyst and an organic cobalt catalyst.
7. The process for preparing an anti-fog automotive lamp silicone sealant according to any one of claims 1 to 6, characterized by comprising the steps of:
adding alkoxy-terminated 107 silicon rubber and calcium powder with different viscosities, fumed silica and carbon slurry into a kneader, kneading at the temperature of 130-150 ℃ and the pressure of-0.09-0.095 MPa to prepare a base material, cooling to normal temperature, and storing in a sealed manner for later use;
step two, adding the base material into a high-speed dispersion machine, evacuating and defoaming, adding the macromolecular cross-linking agent, keeping the vacuum and stirring, and keeping the vacuum to be less than-0.08 MPa in the process;
step three, adding a coupling agent, keeping the air and stirring, and keeping the vacuum to be less than-0.08 MPa;
and step four, adding a catalyst, evacuating, dispersing at a high speed for 30 minutes, and packaging to obtain the product.
8. The preparation method of the anti-fog silicone sealant for automobile lamps according to claim 7, characterized in that:
the relative humidity of the mixing environment in the first step to the fourth step is lower than 70 percent;
kneading for 4 hours in the first step to prepare a base material;
in the second step, the vacuumizing and defoaming time is 10 minutes, and the air-holding and stirring time is 20 minutes;
the air-holding stirring time in the third step is 20 minutes.
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| EP3874002A4 (en) * | 2018-10-31 | 2022-06-01 | Dow Silicones Corporation | Adhesive |
| CN111019593B (en) * | 2019-12-23 | 2021-11-30 | 成都硅宝科技股份有限公司 | Equal-proportion mixed organosilicon sealant for anti-fog car lamp and preparation method thereof |
| CN111621016B (en) * | 2020-06-12 | 2022-06-24 | 北京天山新材料技术有限公司 | Organic silicon polymer and preparation method thereof, adhesive and application thereof |
| CN115505367B (en) * | 2022-09-15 | 2023-03-17 | 成都高新区今天硅材料有限公司 | High-strength organic silicon adhesive and preparation method thereof |
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