CN107118736B - Dealcoholized organosilicon sealant composition, dealcoholized organosilicon sealant and preparation method thereof - Google Patents
Dealcoholized organosilicon sealant composition, dealcoholized organosilicon sealant and preparation method thereof Download PDFInfo
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- CN107118736B CN107118736B CN201610105422.4A CN201610105422A CN107118736B CN 107118736 B CN107118736 B CN 107118736B CN 201610105422 A CN201610105422 A CN 201610105422A CN 107118736 B CN107118736 B CN 107118736B
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- 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
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- 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
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- 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
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- 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
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- 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
- C09J11/08—Macromolecular additives
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/10—Transparent films; Clear coatings; Transparent materials
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- 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
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Abstract
The invention relates to the field of sealants, and discloses a dealcoholized organosilicon sealant composition, which comprises the following components in part by weight: the composite material comprises alkoxy-terminated polydimethylsiloxane, white carbon black, an organic tin catalyst, a plasticizer, a water removing agent, a tackifier and a stabilizer, wherein the plasticizer is methyl silicone oil; the tackifier is one or more of a bisaminosilane tackifier, a monoaminosilane tackifier and an alkoxy silane tackifier; the stabilizer is alkyl trialkoxysilane. The invention also provides a method for preparing the dealcoholized organosilicon sealant by adopting the composition, and the dealcoholized organosilicon sealant prepared by the dealcoholized organosilicon sealant. The dealcoholized organosilicon sealant prepared by the composition can obtain better mechanical property and system stability under the condition of ensuring better transparency.
Description
Technical Field
The invention relates to the field of sealants, in particular to a dealcoholized organosilicon sealant composition, a dealcoholized organosilicon sealant and a preparation method thereof.
Background
At present, the transparent dealcoholized silica gel products on the market are few, and the traditional dealcoholized silica gel is prepared by taking hydroxyl-terminated polydimethylsiloxane as a base rubber and adding proper reinforcing filler (calcium carbonate, silicon dioxide, organic montmorillonite and the like), crosslinking agent (methyltrimethoxysilane, vinyltrimethoxysilane, methyltriethoxysilane and the like) and catalyst (organic titanium catalyst such as ethyl titanate, propyl titanate and the like or organic tin catalyst such as n-butyl tin dilaurate, stannous oxalate and the like). Alternatively, alkoxy-terminated polydimethylsiloxanes are used as the base rubber, with appropriate reinforcing fillers (calcium carbonate, silica, organo montmorillonite, etc.), catalysts (organic titanium catalysts such as ethyl titanate, propyl titanate, etc., or organic tin catalysts such as n-butyl tin dilaurate, stannous oxalate, etc.). However, the existing products have the defects of poor mechanical property, unsatisfactory bonding property, poor system stability, poor yellowing resistance and aging resistance and the like. In particular, the mechanical property and the system stability mainly influence the marketization of the transparent dealcoholized silica gel product. The poor mechanical property is because the larger the filling amount is, the poorer the transparency of the dealcoholized silica gel is, and the poor the adhesion property is, in order to ensure that the transparency of the dealcoholized silica gel is the inorganic filler which can not be added with too much reinforcement, even if the dealcoholized silica gel is white carbon black with better transparency; the reason why the stability of the system is poor is that a plurality of micromolecular substances with different activities exist in the dealcoholized silica gel, and the micromolecular substances can generate a series of reactions along with the lapse of time, so that the content of each component in the system is changed, and the dealcoholized silica gel has the situations of viscosity reduction, yellowing, extrusion, solidification incapability and the like.
Disclosure of Invention
The invention aims to provide a dealcoholized organosilicon sealant composition with better mechanical property and system stability, a dealcoholized organosilicon sealant and a preparation method thereof, aiming at the defects of poorer mechanical property and system stability of a transparent dealcoholized organosilicon sealant.
In order to achieve the above object, the present invention provides a dealcoholized silicone sealant composition comprising: the composite material comprises alkoxy-terminated polydimethylsiloxane, white carbon black, an organic tin catalyst, a plasticizer, a water removing agent, a tackifier and a stabilizer, wherein the plasticizer is methyl silicone oil; the tackifier is one or more of a bisaminosilane tackifier, a monoaminosilane tackifier and an alkoxy silane tackifier; the stabilizer is alkyl trialkoxysilane.
The invention also provides a preparation method of the dealcoholized organosilicon sealant, which comprises the step of mixing the components contained in the composition.
The invention also provides the dealcoholized organosilicon sealant prepared by the method.
The dealcoholized organosilicon sealant prepared by the composition can obtain better mechanical property and system stability under the condition of ensuring better transparency.
Additional features and advantages of the invention will be set forth in the detailed description which follows.
Detailed Description
The following describes in detail specific embodiments of the present invention. It should be understood that the detailed description and specific examples, while indicating the present invention, are given by way of illustration and explanation only, not limitation.
The invention provides a dealcoholized organosilicon sealant composition, which comprises the following components in part by weight: the composite material comprises alkoxy-terminated polydimethylsiloxane, white carbon black, an organic tin catalyst, a plasticizer, a water removing agent, a tackifier and a stabilizer, wherein the plasticizer is methyl silicone oil; the tackifier is one or more of a bisaminosilane tackifier, a monoaminosilane tackifier and an alkoxy silane tackifier; the stabilizer is alkyl trialkoxysilane.
According to the invention, in order to obtain better mechanical properties and system stability under the condition of ensuring better transparency, preferably, relative to 100 parts by weight of alkoxy-terminated polydimethylsiloxane, the white carbon black is used in an amount of 5-25 parts by weight, the organic tin catalyst is used in an amount of 0.1-1 part by weight, the plasticizer is used in an amount of 10-40 parts by weight, the water scavenger is used in an amount of 0.5-5 parts by weight, the tackifier is used in an amount of 0.5-5 parts by weight, and the stabilizer is used in an amount of 1-6 parts by weight.
More preferably, the white carbon black is used in an amount of 10 to 25 parts by weight, the organotin catalyst is used in an amount of 0.2 to 1 part by weight, the plasticizer is used in an amount of 15 to 35 parts by weight, the water scavenger is used in an amount of 0.5 to 2 parts by weight, the tackifier is used in an amount of 0.5 to 2 parts by weight, and the stabilizer is used in an amount of 2 to 5 parts by weight, based on 100 parts by weight of the alkoxy-terminated polydimethylsiloxane.
Still more preferably, the white carbon black is used in an amount of 15 to 22 parts by weight, the organotin catalyst is used in an amount of 0.2 to 0.5 part by weight, the plasticizer is used in an amount of 15 to 25 parts by weight, the water scavenger is used in an amount of 1 to 2 parts by weight, the tackifier is used in an amount of 1 to 2 parts by weight, and the stabilizer is used in an amount of 3 to 5 parts by weight, based on 100 parts by weight of the alkoxy-terminated polydimethylsiloxane.
According to the present invention, the alkoxy-terminated polydimethylsiloxane may employ various alkoxy-terminated polydimethylsiloxanes conventionally used in the art for the preparation of silicone sealants. Specific examples of the alkoxy-terminated polydimethylsiloxane may be, for example: one or more of dimethoxy terminated polydimethylsiloxane, trimethoxy terminated polydimethylsiloxane, and triethoxy terminated polydimethylsiloxane.
It is preferable to use an alkoxy-terminated polydimethylsiloxane having an apparent viscosity of 2000-40000 mPas (more preferably 8000-35000 mPas, still more preferably 10000-35000 mPas).
According to the present invention, the silica is preferably fumed silica, and more preferably fumed silica with a surface modified, for example, one or more of fumed silica with a dimethyldichlorosilane surface modified, fumed silica with a hexamethyldisilazane surface modified, and the like. The surface-modified fumed silica can be a commercially available product or can be prepared by a conventional method in the field, and is not described herein again.
According to the invention, the organic tin catalyst can catalyze the wetting curing of organic silicon, preferably, the organic tin catalyst is one or more of di-n-butyl tin dilaurate, stannous oxalate and stannous octoate, and more preferably, is di-n-butyl tin dilaurate.
According to the invention, the tackifier has the effects of increasing the bonding performance and helping curing and crosslinking, and can be matched with other components in the composition to obtain the transparent dealcoholized organosilicon sealant with improved transparency and excellent mechanical property and system stability. The tackifier is one or more of a bisaminosilane tackifier, a monoaminosilane tackifier and an alkoxy silane tackifier.
The specific example of the bisaminosilane adhesion promoter may be N- (β -aminoethyl) -gamma-aminopropyltrimethoxysilane.
Specific examples of the monoaminosilane adhesion promoter may be, for example: gamma-aminopropyltrimethoxysilane.
Specific examples of the alkoxysilane adhesion promoter may be, for example: gamma- (2, 3-epoxypropoxy) propyltrimethoxysilane.
Preferably, the tackifier is one or more of N- (β -aminoethyl) -gamma-aminopropyltrimethoxysilane, gamma-aminopropyltrimethoxysilane and gamma- (2, 3-epoxypropoxy) propyltrimethoxysilane, and particularly preferably N- (β -aminoethyl) -gamma-aminopropyltrimethoxysilane (H)2N(CH2)2NH(CH2)3Si(OCH3)3)。
In the invention, the organotin catalyst and the adhesion promoter have a certain coordination effect, and the weight ratio of the organotin catalyst to the adhesion promoter is preferably 100: 400-600, more preferably 100: 450-550. When the weight ratio of the organotin catalyst to the tackifier is within the above range, a dealcoholized silicone sealant having more excellent performance can be obtained. Particularly for the matching of an organic tin catalyst and a bisaminosilane tackifier, the activity of the organic tin catalyst is higher, and if the addition amount is increased for the quick surface drying of the sealant, the surface drying time is shortened, and the deep curing of the sealant is promoted, which brings some adverse effects to the storage of the sealant, and because the organic tin is harmful to the environment, the addition amount is strictly limited, and when the bisaminosilane tackifier with certain catalysis promotion function and the organic tin catalyst are compounded and used in a proper proportion, the deep curing can not be excessively influenced while the quick surface drying is ensured, so that the dealcoholized organosilicon sealant with better storage stability can be obtained. Therefore, the composition of the present invention more preferably contains, by weight, 100: 450-550 organotin catalysts and bisaminosilane adhesion promoters.
According to the invention, the plasticizer has the effects of diluting the whole composition system and increasing the elastoplasticity of the sealant, and can be matched with other components in the composition to obtain the transparent dealcoholized organosilicon sealant with improved transparency and excellent mechanical property and system stability, and the plasticizer is methyl silicone oil, preferably the methyl silicone oil with the apparent viscosity of 100-2000mPa & s. When the methyl silicone oil with the apparent viscosity of 100-2000 mPas is used as the plasticizer, the methyl silicone oil in the viscosity range can be well dispersed between macromolecules, white carbon black and the like, so that relative sliding can be easily generated during deformation, the obtained dealcoholized silicone sealant can obtain better elasticity and deformation capability, and a better sealing effect can be obtained.
According to the invention, the water removing agent removes water through reaction with water in a composition system, and can be mixed with other components in the composition to obtain the transparent dealcoholization type organosilicon sealant with improved transparency and excellent mechanical property and system stability.
According to the invention, the alkyl trialkoxysilane used as the stabilizer has higher reaction activity, can react with small molecular substances in a dealcoholized silicon organosilicon sealant composition system, reduces other excessive side reactions, and reduces the possibility of the problems of viscosity reduction, yellowing and the like of the system; the dealcoholized silicone sealant can be smoothly cured and the whole system is more stable. Preferably, the stabilizer is one or more of methyltrimethoxysilane, ethyltrimethoxysilane, methyltriethoxysilane, and ethyltriethoxysilane, more preferably methyltrimethoxysilane.
The invention also provides a preparation method of the dealcoholized organosilicon sealant, which comprises the step of mixing the components contained in the composition.
Although the method of the present invention may include a method of mixing the components contained in the above composition in any form, for example, a method of mixing the components contained in the above composition at once, or a method of mixing them in a certain order may be employed, wherein, for the method of mixing at once, the method comprises: mixing alkoxy-terminated polydimethylsiloxane, white carbon black, an organic tin catalyst, a plasticizer, a water removing agent, a tackifier and a stabilizer.
The conditions for this mixing may include, for example: mixing at 80-150 deg.C and 500-1000rpm for 500-300 min, and then mixing at 15-40 deg.C and 500-1000rpm for 10-60 min. The method further comprises the step of carrying out vacuum defoamation on the mixed product, wherein the conditions of the vacuum defoamation can comprise the following steps: the vacuum degree is between-0.1 MPa and-0.05 MPa, and the defoaming is carried out for 8 to 30min at the temperature of between 15 and 40 ℃ and the rotating speed of 1000 rpm.
Preferably, the dealcoholized silicone sealant of the present invention is prepared by mixing the components contained in the above composition in a certain order, that is, preferably, the method comprises:
(1) mixing alkoxy-terminated polydimethylsiloxane, a plasticizer and a water removal agent;
(2) mixing the product obtained in the step (1) with white carbon black;
(3) mixing the product obtained in the step (2) with a tackifier;
(4) mixing the product obtained in the step (3), an organic tin catalyst and a stabilizer.
According to the present invention, the alkoxy-terminated polydimethylsiloxane, the white carbon black, the organotin catalyst, the plasticizer, the water scavenger, the tackifier and the stabilizer are used in the above-mentioned types and amounts, and are not described herein again.
According to the present invention, it is preferable that the mixing conditions of step (1) include: the temperature is 90-150 deg.C (preferably 100-120 deg.C), and the time is 30-90min (preferably 40-60 min). The mixing may be carried out at a stirring rate of 300-. The mixing in this step serves the purpose of removing water and can be carried out in various ways conventional in the art, for example, in a dynamic mixer.
According to the present invention, in step (2), the silica is preferably dried at a high temperature, for example, at 100-150 ℃ for 12-30h before mixing. Preferably, the mixing conditions of step (2) include: the temperature is 90-150 deg.C (preferably 100-120 deg.C), and the time is 30-300min (preferably 100-300 min). The mixing may be carried out at a stirring rate of 600-. More preferably, before the mixing in step (2), the product obtained in step (1) and the white carbon black are subjected to vacuum defoaming treatment under the following conditions: the vacuum degree is between-0.1 MPa and-0.05 MPa, the stirring speed is between 300 and 1000rpm (preferably between 500 and 900rpm), the temperature is between 80 and 150 ℃ (preferably between 90 and 120 ℃), and the time is between 10 and 60min (preferably between 20 and 40 min); or mixing the product obtained in the step (1) and the white carbon black at the same time of performing the step (2) to perform vacuum defoaming treatment. The former is preferably used.
According to the present invention, preferably, the mixing conditions of step (3) include: the temperature is 10-40 deg.C (preferably 25-40 deg.C), and the time is 10-60min (preferably 20-30 min). The mixing may be carried out at a stirring rate of 300-1000rpm, preferably 500-900 rpm. This step mixing is preferably performed in an inert gas atmosphere, and may be performed in an inert gas atmosphere of one or more of nitrogen, helium, and neon, for example. The dispersion treatment in the inert gas atmosphere can advantageously shorten the following time for the vacuum defoaming treatment.
According to the present invention, preferably, the mixing conditions of step (4) include: the temperature is 10-40 deg.C (preferably 25-40 deg.C), and the time is 10-60min (preferably 20-30 min). The mixing may be carried out at a stirring rate of 300-1000rpm, preferably 500-900 rpm. More preferably, the method comprises: after the mixing in step (4) is performed, the product obtained by the mixing is subjected to a defoaming treatment. The product obtained by mixing in the step (4) can be sent to a vacuum defoaming machine for defoaming, and the defoaming treatment conditions comprise: the vacuum degree is between-0.1 MPa and-0.05 MPa, the stirring speed is between 300 and 1000rpm (preferably between 500 and 900rpm), the temperature is between 10 and 40 ℃ (preferably between 25 and 40 ℃), and the time is between 10 and 60min (preferably between 10 and 30 min).
Of course, the dealcoholized silicone sealants of the present invention do not exclude other additive ingredients as long as such additive ingredients do not affect the performance of the dealcoholized silicone sealants obtained in the present invention. Such an additive may be, for example, white mineral oil. These additives may be added and mixed in any of the above-mentioned steps as long as such addition does not affect the performance of the dealcoholized silicone sealant obtained in the present invention.
The invention also provides the dealcoholized organosilicon sealant prepared by the method. The dealcoholized organosilicon sealant has good transparency, mechanical property and system stability. The surface drying time period is short, the curing speed is high, the bonding strength is high, and the dealcoholized organosilicon sealant is excellent.
The present invention will be described in detail below by way of examples.
In the following examples:
the dimethyldichlorosilane surface treated fumed silica was purchased under the trade designation AEROSILR974 from EVONIK-DEGUSSA.
Example 1
This example illustrates the dealcoholized silicone sealant compositions and dealcoholized silicone sealants of the present invention and methods of making the same.
(1) 1000g of dimethoxy-terminated polydimethylsiloxane (available from Jiangsuchuan new materials Co., Ltd., brand F-40A, apparent viscosity of 35000 mPas, hereinafter the same), 200g of methyl silicone oil (available from Guangzhou Asiatic chemical Co., Ltd., trade name YT-MS100, apparent viscosity of 100 mPas, hereinafter the same) and 10g of vinyltrimethoxysilane were added to a power mixer, and stirred at 120 ℃ and 900rpm for 60min, thereby mixing and removing water;
(2) feeding the product obtained in the step (1) into a vacuum defoaming machine, adding 200g of gas-phase white carbon black (the white carbon black is dried at 120 ℃ for 24 hours in advance) subjected to surface treatment by using dimethyldichlorosilane, stirring and defoaming for 30 minutes at the vacuum degree of-0.06 MPa and the temperature of 120 ℃ and at the rotating speed of 900rpm, feeding the product into a power mixer, and stirring for 300 minutes at the normal pressure and the temperature of 120 ℃ and at the rotating speed of 1500 rpm;
(3) cooling the product obtained in step (2) to room temperature (about 25 ℃) and adding 10g of N- (β -aminoethyl) - γ -aminopropyltrimethoxysilane under a nitrogen atmosphere and stirring at 900rpm for 20min at room temperature (about 25 ℃);
(4) adding 2g of di-n-butyl tin dilaurate and 30g of methyltrimethoxysilane into the product obtained in the step (3), stirring at the rotation speed of 900rpm for 20min at room temperature (about 25 ℃), then feeding the product into a vacuum defoaming machine, stirring and defoaming at the rotation speed of 900rpm at the vacuum degree of-0.06 MPa at 30 ℃ for 10min, and discharging to obtain a sealant A1.
Example 2
This example illustrates the dealcoholized silicone sealant compositions and dealcoholized silicone sealants of the present invention and methods of making the same.
Sealant A2 was prepared according to the method described in example 1, except that 180g of methyl silicone oil, 9g of vinyltrimethoxysilane, 180g of dimethyldichlorosilane surface treated fumed silica, and 9g of N- (β -aminoethyl) - γ -aminopropyltrimethoxysilane were used.
Example 3
This example illustrates the dealcoholized silicone sealant compositions and dealcoholized silicone sealants of the present invention and methods of making the same.
Sealant A3 was prepared according to the method described in example 1, except that 210g of methyl silicone oil, 11g of vinyltrimethoxysilane, 210g of dimethyldichlorosilane surface treated fumed silica, and 11g of N- (β -aminoethyl) - γ -aminopropyltrimethoxysilane were used.
Example 4
This example illustrates the dealcoholized silicone sealant compositions and dealcoholized silicone sealants of the present invention and methods of making the same.
Sealant A4 was obtained according to the procedure as described in example 1, except that stannous oxalate was used instead of di-n-butyl tin dilaurate, and triethoxy-terminated polydimethylsiloxane (available from Jiangsuchoxin New materials corporation, trade name E-51, apparent viscosity 3000 mPas) was used instead of dimethoxy-terminated polydimethylsiloxane.
Example 5
This example illustrates the dealcoholized silicone sealant compositions and dealcoholized silicone sealants of the present invention and methods of making the same.
Sealant A5 was prepared according to the procedure described in example 1, except that N- (β -aminoethyl) - γ -aminopropyltrimethoxysilane was used in an amount of 8 g.
Example 6
This example illustrates the dealcoholized silicone sealant compositions and dealcoholized silicone sealants of the present invention and methods of making the same.
Sealant A6 was prepared according to the procedure described in example 1, except that N- (β -aminoethyl) - γ -aminopropyltrimethoxysilane was used in an amount of 12 g.
Example 7
This example illustrates the dealcoholized silicone sealant compositions and dealcoholized silicone sealants of the present invention and methods of making the same.
According to the method described in example 1, except that all the components used in example 1 were stirred together at 120 ℃ and 900rpm for 410min, further stirred at 900rpm for 20min at room temperature (about 25 ℃), stirred and defoamed at 30 ℃ and 30 ℃ under a vacuum of-0.06 MPa for 10min, and sealant A7 was obtained.
Example 8
This example illustrates the dealcoholized silicone sealant compositions and dealcoholized silicone sealants of the present invention and methods of making the same.
Sealant A8 was prepared according to the procedure described in example 1, except that gamma-aminopropyltrimethoxysilane was used in place of N- (β -aminoethyl) -gamma-aminopropyltrimethoxysilane.
Comparative example 1
Sealant D1 was prepared according to the procedure described in example 1 except that methyltrimethoxysilane was not added in step (4).
Comparative example 2
Sealant D2 was prepared according to the procedure described in example 1, except that propyl titanate was used in place of di-N-butyl tin dilaurate and the silane coupling agent gamma-aminopropyltrimethoxysilane was used in place of N- (β -aminoethyl) -gamma-aminopropyltrimethoxysilane.
Test example
The tack free time, cure rate, tensile strength, elongation at break, Al-Al bond strength, light transmittance, hardness, and pot life of the above sealants A1-A8 and D1-D2 were measured and are shown in Table 1, wherein:
the method for measuring the surface dry time comprises the following steps: coating a proper amount of sealant on a clean polytetrafluoroethylene plate at the temperature of (25 +/-5) DEG C and the RH of (55 +/-5)% to obtain a thickness of about 2mm, and lightly touching the surface of the sealant with fingers every 1min until the sealant is not sticky, wherein the surface drying time is the time for tack-free;
the method for measuring the curing speed comprises the following steps: a Teflon taper slot about 300mm in length and 0-10mm deep is used. Extruding a proper amount of sealant into a chute, leveling by a scraper, standing at 25 + -2 deg.C and 55 + -5% RH for 24h without bubbles in the sealant layer, peeling off the sealant film from the thinnest part to the uncured adhesive part, and measuring the depth of the groove at mm/24 h.
The tensile strength and elongation at break were measured according to the method described in GB/T528-1998;
the Al-Al bond strength was measured according to the method described in GB/T7124-2008;
the light transmittance is tested according to the specification in the standard GB/T2410-2008 'determination of light transmittance and haze of transparent plastics', and the thickness of the film is 1 mm;
hardness was measured according to the method described in GB/T531-1999;
the method for measuring the storage period comprises the following steps: the sealed tube filled with the transparent dealcoholized sealant is placed in a dark and dry environment at 25 ℃ for storage, samples are taken periodically (about 1 month), the appearance state of the sealant is observed by extrusion, and the mechanical properties (namely the tensile strength and the elongation at break) of the sealant are tested (according to the detection experiment), the critical time when the appearance state and the properties are not changed greatly and the normal storage period are obtained.
TABLE 1
As can be seen from the data in table 1, when the dealcoholized silicone sealant composition of the present invention is used to prepare the dealcoholized silicone sealant, the dealcoholized silicone sealant having good elasticity and strength and good storage stability can be obtained, for example, the surface drying time is less than 20min, preferably less than 10min, and more preferably 2-5 min; the curing speed is more than 4.5mm/24h, preferably 6-7mm/24 h; a tensile strength of 1.3MPa or more, preferably 1.9MPa or more; the elongation at break is more than 200%, preferably about 300-380%; the bonding strength of Al-Al is more than 1.2MPa, preferably 1.7-2 MPa; the light transmittance is more than 80%, preferably more than 90%; the hardness is Shore A of 15-25; the storage period is more than 3 months, preferably more than 6 months.
The preferred embodiments of the present invention have been described in detail, however, the present invention is not limited to the specific details of the above embodiments, and various simple modifications may be made to the technical solution of the present invention within the technical idea of the present invention, and these simple modifications are within the protective scope of the present invention.
It should be noted that the various technical features described in the above embodiments can be combined in any suitable manner without contradiction, and the invention is not described in any way for the possible combinations in order to avoid unnecessary repetition.
In addition, any combination of the various embodiments of the present invention is also possible, and the same should be considered as the disclosure of the present invention as long as it does not depart from the spirit of the present invention.
Claims (19)
1. A dealcoholized silicone sealant composition comprising: the composite material comprises alkoxy-terminated polydimethylsiloxane, white carbon black, an organic tin catalyst, a plasticizer, a water removing agent, a tackifier and a stabilizer, wherein the plasticizer is methyl silicone oil; the tackifier is one or more of a bisaminosilane tackifier, a monoaminosilane tackifier and an alkoxy silane tackifier; the stabilizer is alkyl trialkoxysilane;
the preparation method comprises the following steps of (1) relative to 100 parts by weight of alkoxy-terminated polydimethylsiloxane, 15-22 parts by weight of white carbon black, 0.2-0.5 part by weight of organic tin catalyst, 15-25 parts by weight of plasticizer, 1-2 parts by weight of water removing agent, 1-2 parts by weight of tackifier and 3-5 parts by weight of stabilizer; the weight ratio of the organotin catalyst to the tackifier is 100: 400-600.
2. The composition of claim 1 wherein the weight ratio of the organotin catalyst to the adhesion promoter is 100: 450-550.
3. The composition of claim 1 or 2, wherein the organotin catalyst is one or more of di-n-butyl tin dilaurate, stannous oxalate and stannous octoate.
4. The composition of claim 3 wherein the organotin catalyst is di-n-butyl tin dilaurate.
5. The composition as claimed in claim 1 or 2, wherein the plasticizer is a methyl silicone oil having an apparent viscosity of 100-2000 mPa-s.
6. The composition of claim 1 or 2, wherein the water scavenger is one or more of vinyltrimethoxysilane, anhydrous calcium chloride and calcium oxide.
7. The composition of claim 6, wherein the water scavenger is vinyltrimethoxysilane.
8. The composition of claim 1 or 2, wherein the adhesion promoter is one or more of N- (β -aminoethyl) - γ -aminopropyltrimethoxysilane, and γ - (2, 3-epoxypropoxy) propyltrimethoxysilane.
9. The composition of claim 8, wherein the adhesion promoter is N- (β -aminoethyl) - γ -aminopropyltrimethoxysilane.
10. The composition of claim 1 or 2, wherein the stabilizer is one or more of methyltrimethoxysilane, ethyltrimethoxysilane, methyltriethoxysilane, and ethyltriethoxysilane.
11. A method of preparing a dealcoholized silicone sealant comprising mixing the ingredients contained in the composition of any one of claims 1 to 10.
12. The method of claim 11, wherein the method comprises:
(1) mixing alkoxy-terminated polydimethylsiloxane, a plasticizer and a water removal agent;
(2) mixing the product obtained in the step (1) with white carbon black;
(3) mixing the product obtained in the step (2) with a tackifier;
(4) mixing the product obtained in the step (3), an organic tin catalyst and a stabilizer.
13. The method of claim 12, wherein the mixing conditions of step (1) comprise: the temperature is 90-150 deg.C, and the time is 30-90 min.
14. The method of claim 12, wherein the mixing conditions of step (2) comprise: the temperature is 90-150 deg.C, and the time is 30-300 min.
15. The method of claim 12, wherein the mixing conditions of step (3) comprise: the temperature is 10-40 deg.C, and the time is 10-60 min.
16. The method of claim 12, wherein the mixing conditions of step (4) comprise: the temperature is 10-40 deg.C, and the time is 10-60 min.
17. The method of any of claims 12-16, wherein the method further comprises: before mixing in the step (2), defoaming the product obtained in the step (1) and white carbon black; or mixing the product obtained in the step (1) and the white carbon black and defoaming the product while mixing the product in the step (2).
18. The method of any of claims 12-16, wherein the method further comprises: after the mixing in step (4) is performed, the product obtained by the mixing is subjected to a defoaming treatment.
19. A dealcoholized silicone sealant prepared according to the method of any one of claims 11 to 18.
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| CN201610105422.4A CN107118736B (en) | 2016-02-25 | 2016-02-25 | Dealcoholized organosilicon sealant composition, dealcoholized organosilicon sealant and preparation method thereof |
| PCT/CN2017/074623 WO2017143997A1 (en) | 2016-02-25 | 2017-02-23 | Dealcoholised organic silicon sealant composition and preparation method therefor |
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| CN201610105422.4A CN107118736B (en) | 2016-02-25 | 2016-02-25 | Dealcoholized organosilicon sealant composition, dealcoholized organosilicon sealant and preparation method thereof |
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| CN107118736A CN107118736A (en) | 2017-09-01 |
| CN107118736B true CN107118736B (en) | 2020-04-24 |
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| CN108059945B (en) * | 2017-12-30 | 2020-11-10 | 广州市白云化工实业有限公司 | Organosilicon sealant for photovoltaic dual-glass assembly and preparation method thereof |
| CN110305619A (en) * | 2019-05-23 | 2019-10-08 | 宁波聚力新材料科技有限公司 | Translucent food grade is bonded and sealed glue |
| CN110591638B (en) * | 2019-11-04 | 2021-10-19 | 镇江博慎新材料有限公司 | Low-proportion bi-component dealcoholized organosilicon sealant and preparation method and application thereof |
| CN111320964A (en) * | 2020-03-20 | 2020-06-23 | 佛山市金云信硅材料制品有限公司 | Silicone sealant and preparation method thereof |
| CN111961346B (en) * | 2020-09-01 | 2021-07-13 | 北京理工大学 | A kind of silicone rubber composite material with both high strength and adhesion properties and preparation method thereof |
| CN113072809B (en) * | 2021-03-24 | 2022-11-01 | 深圳市新亚电子制程股份有限公司 | Single-component vulcanized silicone rubber and preparation method and application thereof |
| CN113930205B (en) * | 2021-10-28 | 2023-08-15 | 广州集泰化工股份有限公司 | Sealant for refrigerated container |
| CN114874747B (en) * | 2022-05-05 | 2023-01-03 | 安徽斯迈特新材料股份有限公司 | Preparation method of high-temperature-resistant and strong-ultraviolet-resistant MS (Murashige & Skoog) adhesive |
| CN114958291B (en) * | 2022-06-09 | 2023-07-04 | 北京航空材料研究院股份有限公司 | Single-component high-adhesion room temperature vulcanized organosilicon sealant and preparation method thereof |
| CN115521755B (en) * | 2022-08-29 | 2023-07-07 | 湖北武大光子科技有限公司 | Caulking silicone sealant special for ballastless track of high-speed railway and preparation method thereof |
| CN115216268B (en) * | 2022-09-02 | 2023-08-18 | 江西蓝星星火有机硅有限公司 | Dealcoholized transparent high-fluidity organic silicon sealant and preparation method thereof |
| CN115584238A (en) * | 2022-11-28 | 2023-01-10 | 唐山三孚纳米材料有限公司 | Pure white sealant prepared from single-component room temperature vulcanized silicone rubber and preparation method thereof |
| CN115725261A (en) * | 2022-12-12 | 2023-03-03 | 江苏中恒电子新材料有限公司 | Organic silicon sealant for preventing electric heating element from being damp and preparation method thereof |
| CN116042172A (en) * | 2023-02-02 | 2023-05-02 | 江西晨光新材料股份有限公司 | Single-component dealcoholized room temperature vulcanized silicone rubber and preparation method thereof |
| CN117210192B (en) * | 2023-09-13 | 2024-11-12 | 江西蓝星星火有机硅有限公司 | One-component alcohol-free organic silicon sealant composition and preparation method thereof |
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