WO2017143997A1 - 脱醇型有机硅密封胶组合物及其制备方法 - Google Patents

脱醇型有机硅密封胶组合物及其制备方法 Download PDF

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WO2017143997A1
WO2017143997A1 PCT/CN2017/074623 CN2017074623W WO2017143997A1 WO 2017143997 A1 WO2017143997 A1 WO 2017143997A1 CN 2017074623 W CN2017074623 W CN 2017074623W WO 2017143997 A1 WO2017143997 A1 WO 2017143997A1
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tackifier
weight
mixing
amount
parts
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PCT/CN2017/074623
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English (en)
French (fr)
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徐斌
张玲玲
林信平
李跳南
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比亚迪股份有限公司
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Publication of WO2017143997A1 publication Critical patent/WO2017143997A1/zh

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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
    • 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
    • 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
    • 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
    • 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

Definitions

  • the invention relates to the field of sealants, in particular to a dealcoholized silicone sealant composition and a preparation method thereof.
  • an alkoxy-terminated polydimethylsiloxane is used as a base rubber, and a suitable reinforcing filler (calcium carbonate, silica, organic montmorillonite, etc.), a catalyst (organic titanium catalyst such as ethyl titanate) , propyl titanate, etc.; or organotin catalysts, such as n-butyl dilaurate, stannous oxalate, etc.).
  • a suitable reinforcing filler calcium carbonate, silica, organic montmorillonite, etc.
  • a catalyst organic titanium catalyst such as ethyl titanate
  • propyl titanate propyl titanate
  • organotin catalysts such as n-butyl dilaurate, stannous oxalate, etc.
  • the poor mechanical properties are because the transparency of the de-alcoholized silica gel is not added to the reinforcing inorganic filler. Even if the white carbon black has better transparency, the larger the filling amount, the worse the transparency of the de-alcoholized silica gel.
  • the connection performance is not satisfactory; the stability of the system is poor because there are many different active small molecules in the de-alcoholized silica gel. Over time, these small molecules will undergo a series of reactions, making the components of the system The content changes, causing the de-alcoholized silica gel to have a decrease in viscosity, yellowing, and extrusion failure.
  • the object of the present invention is to provide a dealcoholized silicone sealant composition with good mechanical properties and system stability and a preparation method thereof for the defects of poor mechanical properties and stability of the transparent dealcoholized silicone sealant. .
  • the present invention provides a dealcoholized silicone sealant composition
  • a dealcoholized silicone sealant composition comprising: an alkoxy-terminated polydimethylsiloxane, white carbon, in accordance with an embodiment of the present invention a black, organotin catalyst, a plasticizer, a water scavenger, a tackifier, and a stabilizer, wherein the plasticizer is methyl silicone oil; the tackifier is a bisaminosilane tackifier, and a monoaminosilane is added.
  • the stabilizer is an alkyltrialkoxysilane.
  • the dealcoholized silicone sealant according to the embodiment of the present invention can have better mechanical properties and system stability while ensuring better transparency.
  • the invention provides a process for the preparation of a dealcoholized silicone sealant composition.
  • the method comprises: mixing the components contained in the dealcoholized silicone sealant composition described in the previous examples.
  • the dealcoholized silicone sealant composition having better mechanical properties and system stability can be efficiently prepared by the method.
  • the present invention provides a dealcoholized silicone sealant composition
  • a dealcoholized silicone sealant composition comprising: an alkoxy-terminated polydimethylsiloxane, white carbon, in accordance with an embodiment of the present invention Black, organotin catalyst, plasticizer, water scavenger, tackifier and stabilizer, wherein the plasticizer may be methyl silicone oil; the tackifier may be a diaminosilane tackifier, a monoaminosilane tackifier And one or more of the alkoxysilane tackifiers; the stabilizer may be an alkyltrialkoxysilane.
  • the alkoxy-terminated polydimethylsiloxane, the white carbon black may be used in an amount of 5 to 25 parts by weight
  • the organotin catalyst may be used in an amount of 0.1 to 1 part by weight
  • the plasticizer may be used in an amount of 10 to 40 parts by weight.
  • the water-removing agent may be used in an amount of 0.5 to 5 parts by weight
  • the tackifier may be used in an amount of 0.5 to 5 parts by weight
  • the stabilizer may be used in an amount of 1 to 6 parts by weight.
  • the amount of white carbon black may be 10-25 parts by weight relative to 100 parts by weight of the alkoxy-terminated polydimethylsiloxane, and the amount of the organotin catalyst may be used.
  • the amount of the plasticizer may be from 15 to 35 parts by weight
  • the amount of the water removing agent may be from 0.5 to 2 parts by weight
  • the amount of the tackifier may be from 0.5 to 2 parts by weight
  • the amount of the stabilizer is from 0.2 to 1 part by weight. It may be 2 to 5 parts by weight.
  • the amount of white carbon black may be 15-22 parts by weight, based on 100 parts by weight of the alkoxy-terminated polydimethylsiloxane, the amount of the organotin catalyst. It may be 0.2-0.5 parts by weight, the plasticizer may be used in an amount of 15-25 parts by weight, the water removing agent may be used in an amount of 1-2 parts by weight, the tackifier may be used in an amount of 1-2 parts by weight, and the stabilizer may be used. The amount may be 3-5 parts by weight.
  • the alkoxy-terminated polydimethylsiloxane may employ various alkoxy-terminated polydimethylsiloxanes conventionally used in the art for preparing silicone sealants.
  • the alkoxy-terminated polydimethylsiloxane may be dimethoxy-terminated polydimethylsiloxane, trimethoxy-terminated polydimethylsiloxane and three One or more of ethoxylated polydimethylsiloxanes.
  • an alkoxy-terminated polydimethylsiloxane having an apparent viscosity of from 2,000 to 40,000 mPa ⁇ s, more preferably from 8,000 to 35,000 mPa ⁇ s, still more preferably from 10,000 to 35,000 mPa ⁇ s. Oxytomane.
  • the white carbon black is preferably a fumed silica, more preferably a surface modified fumed silica, such as a fumed silica surface modified with dimethyldichlorosilane.
  • a fumed silica such as hexamethyldisilazane surface-modified, fumed silica.
  • the surface-modified fumed silica may be commercially available or may be obtained by a conventional method in the art, and will not be described herein.
  • the organotin catalyst is capable of catalyzing the wet curing of the silicone.
  • the organotin catalyst may be one of tin di-n-butyl dilaurate, stannous oxalate and stannous octoate.
  • the organotin catalyst may be di-n-butyltin dilaurate.
  • the tackifier has an effect of increasing adhesion properties and contributing to curing cross-linking, which is capable of blending with other components in the composition to obtain improved transparency and excellent mechanical properties and system stability.
  • Transparent dealcoholized silicone sealant is one or more of a bisaminosilane tackifier, a monoaminosilane tackifier, and an alkoxysilane tackifier.
  • the bisaminosilane tackifier may be N-( ⁇ -aminoethyl)- ⁇ -aminopropyltrimethoxysilane, and the monoaminosilane tackifier may be ⁇ -aminopropyl
  • the trimethoxysilane, alkoxysilane tackifier may be ⁇ -(2,3-epoxypropoxy)propyltrimethoxysilane.
  • the tackifier may be N-( ⁇ -aminoethyl)- ⁇ -aminopropyltrimethoxysilane, ⁇ -aminopropyltrimethoxysilane and ⁇ -( One or more of 2,3-epoxypropoxy)propyltrimethoxysilane, the tackifier is particularly preferably N-( ⁇ -aminoethyl)- ⁇ - according to a specific embodiment of the present invention.
  • Aminopropyltrimethoxysilane H 2 N(CH 2 ) 2 NH(CH 2 ) 3 Si(OCH 3 ) 3 ).
  • the organotin catalyst and the tackifier have a certain complexing effect.
  • the weight ratio of the organotin catalyst to the tackifier is preferably 100:400-600, according to the present invention. In other embodiments of the invention, the weight ratio of the organotin catalyst to the tackifier is more preferably from 100:450 to 550. When the weight ratio of the organotin catalyst to the tackifier is within the above range, a dealcoholized silicone sealant having more excellent properties can be obtained.
  • the organotin catalyst has high activity, and the addition amount can increase the sealing effect of the sealant, and shorten the dry time of the sealant. Promotes its deep curing, but at the same time it also has some adverse effects on the storage of the sealant. on the other hand, Since organotin is harmful to the environment, its amount is also strictly limited.
  • a bis-aminosilane tackifier having a certain catalytic effect is compounded with an organotin catalyst in a suitable ratio, it can ensure rapid drying without excessively affecting deep curing, thereby achieving storage stability. Better de-alcoholic silicone sealant.
  • the composition of the present invention more preferably contains a combination of an organotin catalyst and a bisaminosilane tackifier in a weight ratio of 100:450 to 550.
  • the plasticizer has a function of diluting the entire composition and increasing the elastoplasticity of the sealant, which is capable of blending with other components in the composition to obtain an improved transparency and excellent mechanical properties and system stability.
  • the transparent dealcoholized silicone sealant may be a methyl silicone oil in the present invention, preferably a methyl silicone oil having an apparent viscosity of 100 to 2000 mPa ⁇ s.
  • methyl silicone oil having an apparent viscosity of 100-2000 mPa ⁇ s as a plasticizer, since the methyl silicone oil of the viscosity range can be well dispersed between the macromolecule and the white carbon black, deformation occurs. The relative sliding can easily occur, which can help the obtained dealcoholized silicone sealant to obtain better elasticity and deformation ability, and can also obtain better sealing effect.
  • the water scavenger can react with moisture in the composition system to remove moisture, and by adding a water scavenger and blending other components in the composition, transparency and mechanical properties can be obtained. And transparent dealcoholized silicone sealant with excellent system stability.
  • the water scavenger may be one or more of vinyltrimethoxysilane, anhydrous calcium chloride, and calcium oxide.
  • the water scavenger may be vinyltrimethoxysilane.
  • the stabilizer may be an alkyltrialkoxysilane, and the inventors have found that the alkyltrialkoxysilane has high reactivity and can be combined with a dealcoholized silicone silicone sealant.
  • the reaction of small molecular substances in the system reduces the occurrence of other excessive side reactions, thereby reducing the possibility of some problems such as viscosity drop and yellowing in the system; and the inventors have also found that alkyltrialkoxysilanes also help During the curing cross-linking reaction, the dealcoholized silicone silicone sealant can be cured smoothly, making the whole system more stable.
  • the alkyltrialkoxysilane may preferably be one of methyltrimethoxysilane, ethyltrimethoxysilane, methyltriethoxysilane, and ethyltriethoxysilane. Or more, more preferably methyltrimethoxysilane. Therefore, the system can be more effectively prevented from having problems such as viscosity drop and yellowing, and the dealcoholized silicone silicone sealant can be cured smoothly and the stability of the system can be improved.
  • the invention provides a process for the preparation of a dealcoholized silicone sealant composition.
  • the method comprises: mixing the components contained in the dealcoholized silicone sealant composition described in the previous examples.
  • the method of the present invention may comprise 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 a time, or a method of mixing in a certain order.
  • the method of one-time mixing may include: mixing an alkoxy-terminated polydimethylsiloxane, white carbon black, an organotin catalyst, a plasticizer, a water-removing agent, a tackifier, and a stabilizer.
  • the above mixing may be carried out by first mixing at a temperature of 80-150 ° C, at a speed of 500-1000 rpm for 300-500 min, and then at a temperature of 15-40 ° C, 500-1000 rpm. Mix for 10 to 60 minutes at the speed.
  • the method further comprises vacuum defoaming the mixed product, and the vacuum degassing conditions may include, for example, a vacuum of -0.1 MPa to -0.05 MPa, a temperature of 15 to 40 ° C, and a rotation speed of 500 to 1000 rpm. Defoaming for 8-30 min. (Speed is the stirring speed)
  • the method for preparing the dealcoholized silicone sealant of the present invention comprises mixing the components contained in the above composition in a certain order, that is, preferably, the above mixing may be carried out according to the following steps. :
  • the alkoxy-terminated polydimethylsiloxane, white carbon black, organotin catalyst, plasticizer, water scavenger, tackifier and stabilizer are classified according to an embodiment of the present invention. And the amount used as described above, and will not be described herein.
  • the mixing conditions of the step (1) include a temperature of 90 to 150 ° C (preferably 100 to 120 ° C) and a time of 30 to 90 min (preferably 40 to 60 min). This mixing can be carried out at a stirring rate of 300 to 1000 rpm, preferably 500 to 900 rpm.
  • the mixing of this step can achieve the purpose of water removal, which can be carried out by various means conventional in the art, such as mixing in a power mixer.
  • the white carbon black is preferably dried at a high temperature before mixing, for example, at 100 to 150 ° C for 12 to 30 hours.
  • the mixing conditions of step (2) include a temperature of 90-150 ° C (preferably 100-120 ° C) and a time of 30-300 min (preferably 100-300 min). This mixing can be carried out at a stirring rate of 600 to 1500 rpm, preferably 800 to 1500 rpm. Thereby, the mixing efficiency and the mixing uniformity can be further improved.
  • the method further comprises: defoaming the mixture of the product obtained in the step (1) and the white carbon black or performing the step before performing the mixing of the step (2).
  • the product obtained in the step (1) and the white carbon black are subjected to a defoaming treatment.
  • the product obtained in the step (1) and the white carbon black are subjected to vacuum defoaming treatment, and the conditions of the vacuum defoaming treatment include: the degree of vacuum is - 0.1MPa to -0.05MPa, a stirring speed of 300-1000 rpm (preferably 500-900 rpm), a temperature of 80-150 ° C (preferably 90-120 ° C), a time of 10-60 min (preferably 20-40 min); or
  • the product obtained in the step (1) and the white carbon black are subjected to vacuum defoaming treatment while performing the mixing of the step (2).
  • the former is preferably employed, whereby it is easier to operate.
  • the mixing conditions of the step (3) include a temperature of 10 to 40 ° C (preferably 25 to 40 ° C) and a time of 10 to 60 min (preferably 20 to 30 min).
  • This mixing can be carried out at a stirring rate of 300 to 1000 rpm, preferably 500 to 900 rpm.
  • This step mixing is preferably carried out in an inert gas atmosphere, for example, in an atmosphere of one or more inert gases such as nitrogen, helium and neon.
  • the mixing conditions of the step (4) include a temperature of 10 to 40 ° C (preferably 25 to 40 ° C) and a time of 10 to 60 min (preferably 20 to 30 min). This mixing can be carried out at a stirring rate of 300 to 1000 rpm, preferably 500 to 900 rpm.
  • the method further comprises the step (5): subjecting the product obtained in step (4) to a defoaming treatment.
  • the conditions of the above defoaming treatment include: a degree of vacuum of -0.1 MPa to -0.05 MPa, a stirring speed of 300-1000 rpm (preferably 500-900 rpm), and a temperature of 10-40 ° C ( It is preferably 25-40 ° C) for a period of 10-60 min (preferably 10-30 min).
  • the dealcoholized silicone sealant of the present invention does not exclude other additive components as long as such additive components do not affect the properties of the dealcoholized silicone sealant obtained by the present invention.
  • Such an additive may be, for example, white mineral oil.
  • These additives may be added in any of the above steps as long as such addition does not affect the properties of the dealcoholized silicone sealant obtained by the present invention.
  • the fumed silica surface treated with dimethyldichlorosilane was purchased from EVONIK-DEGUSSA AEROSIL R974 grade.
  • This embodiment is intended to illustrate the dealcoholized silicone sealant composition of the present invention and a process for the preparation thereof.
  • step (2) The product obtained in the step (1) is sent to a vacuum deaerator, and 200 g of dimethyldichlorosilane surface-treated fumed silica (white carbon black has been previously dried at 120 ° C for 24 h) is added. And defoaming at a vacuum of -0.06 MPa, at 120 ° C, at 900 rpm for 30 min, and then the product is sent to a power mixer, under normal pressure, at 120 ° C, stirring at 1500 rpm for 300 min;
  • step (3) The product obtained in the step (2) is lowered to room temperature (about 25 ° C), and 10 g of N-( ⁇ -aminoethyl)- ⁇ -aminopropyltrimethoxysilane is added under a nitrogen atmosphere at room temperature. (about 25 ° C), stirring at 900 rpm for 20 min;
  • step (3) To the product obtained in the step (3), 2 g of di-n-butyltin dilaurate and 30 g of methyltrimethoxysilane were added, and stirred at 900 rpm for 20 min at room temperature (about 25 ° C). Then, the product was sent to a vacuum defoaming machine, and the mixture was degassed at a vacuum of -0.06 MPa at 30 ° C and stirred at 900 rpm for 10 min to obtain a sealant A1.
  • This embodiment is intended to illustrate the dealcoholized silicone sealant composition of the present invention and a process for the preparation thereof.
  • This embodiment is intended to illustrate the dealcoholized silicone sealant composition of the present invention and a process for the preparation thereof.
  • This embodiment is intended to illustrate the dealcoholized silicone sealant composition of the present invention and a process for the preparation thereof.
  • Example 2 According to the method described in Example 1, except that stannous oxalate is used instead of di-n-butyltin dilaurate, and triethoxy-terminated polydimethylsiloxane (purchased from Jiangsu Kexin New Material Co., Ltd.) is used.
  • This embodiment is intended to illustrate the dealcoholized silicone sealant composition of the present invention and a process for the preparation thereof.
  • This embodiment is intended to illustrate the dealcoholized silicone sealant composition of the present invention and a process for the preparation thereof.
  • This embodiment is intended to illustrate the dealcoholized silicone sealant composition of the present invention and a process for the preparation thereof.
  • Example 1 According to the method described in Example 1, except that all the components used in Example 1 were stirred at 120 ° C for 400 min at 900 rpm, and then stirred at 900 rpm for 20 min at room temperature (about 25 ° C). The mixture was degassed at a vacuum of -0.06 MPa at 30 ° C and stirred at 900 rpm for 10 min to obtain a sealant A7.
  • This embodiment is intended to illustrate the dealcoholized silicone sealant composition of the present invention and a process for the preparation thereof.
  • the method for measuring the dry time includes: applying an appropriate amount of sealant on a clean Teflon plate at (25 ⁇ 5) ° C, (55 ⁇ 5)% RH, the thickness is about 2 mm, and is used every 1 min. The finger touches the rubber surface, and the time until the hand is not sticky is the dry time;
  • the method of measuring the curing speed includes: using a polytetrafluoroethylene chute having a length of about 300 mm and a depth of 0-10 mm. Squeeze a proper amount of sealant into the chute, scrape it with a spatula, do not allow air bubbles in the glue layer, and lift it from the thinnest part after being placed for 24 hours at (25 ⁇ 2) °C, (55 ⁇ 5)% RH. The film, up to the uncured adhesion, is measured for the depth of the groove, expressed in mm/24h.
  • the tensile strength and elongation at break are measured according to the method described in GB/T528-1998;
  • the Al-Al bond strength is measured according to the method described in GB/T7124-2008;
  • the light transmittance is tested according to the provisions of the standard GB/T 2410—2008 “Determination of Transparency and Haze of Transparent Plastics”, and the film thickness is 1 mm;
  • the hardness is measured according to the method described in GB/T531-1999;
  • the storage period is measured by placing a sealed tube containing a clear dealcoholized sealant in a dark and dry environment at 25 ° C, sampling periodically (about 1 month), and observing the appearance of the sealant, and The mechanical properties (ie, tensile strength and elongation at break) were tested (according to the above test), and the critical time of appearance state and performance change was small and its normal storage period.
  • a better dealcoholized silicone sealant for example, a surface dry time of 20 min or less, preferably 10 min or less, more preferably 2-5 min; a curing speed of 4.5 mm / 24 h or more, preferably 6-7 mm / 24 h;
  • the tensile strength is above 1.3 MPa, preferably above 1.9 MPa;
  • the elongation at break is above 200%, preferably between about 300 and 380%;
  • the bond strength of Al-Al is above 1.2 MPa, preferably between 1.7 and 2 MPa; It is 80% or more, preferably 90% or more;
  • the hardness Shore A is 15-25; the storage period is 3 months or more, preferably 6 months or more.

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Inorganic Chemistry (AREA)
  • Sealing Material Composition (AREA)

Abstract

公开了脱醇型有机硅密封胶组合物，该组合物含有：烷氧基封端聚二甲基硅氧烷、白炭黑、有机锡催化剂、增塑剂、除水剂、增粘剂和稳定剂，其中，所述增塑剂为甲基硅油；所述增粘剂为双氨基硅烷增粘剂、单氨基硅烷增粘剂和烷氧基硅烷增粘剂中的一种或多种；所述稳定剂为烷基三烷氧基硅烷。

Description

脱醇型有机硅密封胶组合物及其制备方法 技术领域
本发明涉及密封胶领域，具体涉及脱醇型有机硅密封胶组合物及其制备方法。
背景技术
目前市场上的透明脱醇型硅胶产品较少，传统脱醇型硅胶的制备是以端羟基聚二甲基硅氧烷为基胶，加以适当的补强填料(碳酸钙、二氧化硅、有机蒙脱土等)，交联剂(甲基三甲氧基硅烷、乙烯基三甲氧基硅烷、甲基三乙氧基硅烷等)，催化剂(有机钛催化剂如钛酸乙酯、钛酸丙酯等；或者有机锡催化剂，如正丁基二月桂酸锡、草酸亚锡等)。或者，以烷氧基封端聚二甲基硅氧烷为基胶，加以适当的补强填料(碳酸钙、二氧化硅、有机蒙脱土等)，催化剂(有机钛催化剂如钛酸乙酯、钛酸丙酯等；或者有机锡催化剂，如正丁基二月桂酸锡、草酸亚锡等)。然而，现有的这些产品存在一些力学性能较差，粘接性能不理想，体系稳定性不好，耐黄变老化较差等缺点。特别是力学性能和体系稳定性主要影响着透明脱醇型硅胶产品的市场化。力学性能较差是因为为了保证脱醇硅胶的透明度是不会添加太多补强的无机填料，就算是透明度较好的白炭黑，填充量越大，脱醇硅胶的透明度就越差，粘接性能也不理想；体系稳定性能较差是因为在脱醇硅胶中存在很多不同活性的小分子物质，随着时间的推移这些小分子物质就会发生一系列反应，使体系中各个组分的含量发生变化，造成脱醇硅胶会出现粘度降低，发生黄变，挤出无法固化等一些情况。
因此，现有的脱醇型硅胶产品仍有待改进。
发明内容
本发明的目的在于针对透明脱醇型有机硅密封胶力学性能和体系稳定性较差的缺陷，提供一种力学性能和体系稳定性较好的脱醇型有机硅密封胶组合物及其制备方法。
在本发明的第一方面，本发明提供一种脱醇型有机硅密封胶组合物，根据本发明的实施例，该组合物含有：烷氧基封端聚二甲基硅氧烷、白炭黑、有机锡催化剂、增塑剂、除水剂、增粘剂和稳定剂，其中，所述增塑剂为甲基硅油；所述增粘剂为双氨基硅烷增粘剂、单氨基硅烷增粘剂和烷氧基硅烷增粘剂中的一种或多种；所述稳定剂为烷基三烷氧基硅烷。
由此，根据本发明实施例的脱醇型有机硅密封胶能够在保证较好的透明度的情况下，同时具有较好的力学性能和体系稳定性。
在本发明的第二方面，本发明提出了一种脱醇型有机硅密封胶组合物的制备方法。根据本发明的实施例，该方法包括：将前面实施例所述的脱醇型有机硅密封胶组合物含有的成分进行混合。根据本发明的实施例，采用该方法可以有效地制备得到具有较好的力学性能和体系稳定性的脱醇型有机硅密封胶组合物。
本发明的附加方面和优点将在下面的描述中部分给出，部分将从下面的描述中变得明显，或通过本发明的实践了解到。
具体实施方式
以下对本发明的具体实施方式进行详细说明。应当理解的是，此处所描述的具体实施方式仅用于说明和解释本发明，并不用于限制本发明。
在本发明的第一方面，本发明提供一种脱醇型有机硅密封胶组合物，根据本发明的实施例，该组合物含有：烷氧基封端聚二甲基硅氧烷、白炭黑、有机锡催化剂、增塑剂、除水剂、增粘剂和稳定剂，其中，增塑剂可以为甲基硅油；增粘剂可以为双氨基硅烷增粘剂、单氨基硅烷增粘剂和烷氧基硅烷增粘剂中的一种或多种；稳定剂可以为烷基三烷氧基硅烷。
根据本发明的具体实施例，为了能够保证脱醇型有机硅密封胶组合物获得较好的透明度的情况下，获得较好的力学性能和体系稳定性，优选情况下，相对于100重量份的烷氧基封端聚二甲基硅氧烷，白炭黑的用量可以为5-25重量份，有机锡催化剂的用量可以为0.1-1重量份，增塑剂的用量可以为10-40重量份，除水剂的用量可以为0.5-5重量份，增粘剂的用量可以为0.5-5重量份，稳定剂的用量可以为1-6重量份。
根据本发明的具体实施例，更优选地，相对于100重量份的烷氧基封端聚二甲基硅氧烷，白炭黑的用量可以为10-25重量份，有机锡催化剂的用量可以为0.2-1重量份，增塑剂的用量可以为15-35重量份，除水剂的用量可以为0.5-2重量份，增粘剂的用量可以为0.5-2重量份，稳定剂的用量可以为2-5重量份。
根据本发明的具体实施例，更进一步优选地，相对于100重量份的烷氧基封端聚二甲基硅氧烷，白炭黑的用量可以为15-22重量份，有机锡催化剂的用量可以为0.2-0.5重量份，增塑剂的用量可以为15-25重量份，除水剂的用量可以为1-2重量份，增粘剂的用量可以为1-2重量份，稳定剂的用量可以为3-5重量份。
根据本发明的实施例，烷氧基封端聚二甲基硅氧烷可以采用本领域常规的用于制备有机硅密封胶的各种烷氧基封端聚二甲基硅氧烷。根据本发明的具体实施例，烷氧基封端聚二甲基硅氧烷可以为二甲氧基封端聚二甲基硅氧烷、三甲氧基封端聚二甲基硅氧烷和三乙氧基封端聚二甲基硅氧烷中的一种或多种。
根据本发明的具体实施例，优选采用表观粘度为2000-40000mPa·s(更优选为8000-35000mPa·s，更进一步优选为10000-35000mPa·s)的烷氧基封端聚二甲基硅氧烷。
根据本发明的具体实施例，白炭黑优选采用气相法白炭黑，更优选采用表面改性了的气相法白炭黑，例如采用二甲基二氯硅烷表面改性的气相法白炭黑、六甲基二硅氮烷表面改性的气相法白炭黑等中的一种或多种。其中，表面改性了的气相法白炭黑可以是市售品，也可以采用本领域常规的方法制得，在此不再赘述。
根据本发明的具体实施例，有机锡催化剂能够催化有机硅湿化固化，根据本发明的一些实施例有机锡催化剂可以为二正丁基二月桂酸锡、草酸亚锡和辛酸亚锡中的一种或多种，根据本发明的另一些实施例，有机锡催化剂可以为二正丁基二月桂酸锡。
根据本发明的实施例，所述增粘剂具有增加粘接性能且助于固化交联的作用，其能够配合所述组合物中的其他成分获得透明度提高的且力学性能和体系稳定性优良的透明脱醇型有机硅密封胶。本发明中所述增粘剂为双氨基硅烷增粘剂、单氨基硅烷增粘剂和烷氧基硅烷增粘剂中的一种或多种。其中，根据本发明的具体实施例，双氨基硅烷增粘剂可以为N-(β-氨乙基)-γ-氨丙基三甲氧基硅烷，单氨基硅烷增粘剂可以为γ-氨丙基三甲氧基硅烷，烷氧基硅烷增粘剂可以为γ-(2,3-环氧丙氧基)丙基三甲氧基硅烷。
根据本发明的具体实施例，优选情况下，增粘剂可以为N-(β-氨乙基)-γ-氨丙基三甲氧基硅烷、γ-氨丙基三甲氧基硅烷和γ-(2,3-环氧丙氧基)丙基三甲氧基硅烷中的一种或多种，根据本发明的具体实施例，增粘剂特别优选为N-(β-氨乙基)-γ-氨丙基三甲氧基硅烷(H2N(CH2)2NH(CH2)3Si(OCH3)3)。
在本发明中的具体实施例，有机锡催化剂和增粘剂具有一定的配合作用，根据本发明的一些实施例，有机锡催化剂和增粘剂的重量比优选为100：400-600，根据本发明的另一些实施例，有机锡催化剂和增粘剂的重量比更优选为100：450-550。当有机锡催化剂和增粘剂的重量比在上述范围内时，能够获得性能更为优良的脱醇型有机硅密封胶。特别是对于有机锡催化剂和双氨基硅烷增粘剂的配合来说，有机锡类催化剂活性较高，提高其添加量可以获得密封胶快速表干效果，并且在缩短其表干时间的同时还会促进其深层固化，但是同时是也为密封胶的贮存带了一些不利影响。另一方面， 由于有机锡对环境有害，其添加量也是受的严格限制的。而具有一定助催化作用的双氨基硅烷增粘剂与有机锡催化剂以较为合适的比例复配使用时，在保证仍然能快速表干的同时不会过多的影响深层固化，从而可以获得贮存稳定性更好的脱醇型有机硅密封胶。因此，本发明的组合物更优选含有重量比为100：450-550的有机锡催化剂和双氨基硅烷增粘剂的组合。
根据本发明的实施例，增塑剂具有稀释整个组合物的体系以及增加密封胶弹塑性的作用，其能够配合所述组合物中的其他成分获得透明度提高的且力学性能和体系稳定性优良的透明脱醇型有机硅密封胶，本发明中增塑剂可以为甲基硅油，优选为表观粘度为100-2000mPa·s的甲基硅油。在采用表观粘度为100-2000mPa·s的甲基硅油作为增塑剂的情况下，由于该粘度范围的甲基硅油能够很好地分散在大分子和白炭黑等之间，在发生形变时能很容易的发生相对滑动，能够有助于所得的脱醇型有机硅密封胶获得较好的弹性和形变能力，而且也可以获得较好的密封效果。
根据本发明的实施例，除水剂可以与与组合物体系中的水分发生反应，从而除去水分，通过加入除水剂，配合所述组合物中的其他成分，能够获得透明度提高的且力学性能和体系稳定性优良的透明脱醇型有机硅密封胶。根据本发明的一些实施例，除水剂可以为乙烯基三甲氧基硅烷、无水氯化钙和氧化钙中的一种或多种。根据本发明的另一些实施例，除水剂可以为乙烯基三甲氧基硅烷。由此可以进一步提高脱醇型有机硅密封胶的力学性能和体系稳定性。
根据本发明的具体实施例，稳定剂可以为烷基三烷氧基硅烷，发明人发现，烷基三烷氧基硅烷具有较高的反应活性，进而能够与脱醇型硅有机硅密封胶组合物体系中小分子物质反应，减少了其他过多的副反应发生，从而降低了体系出现粘度下降、黄变等一些问题的可能性；同时发明人还发现，烷基三烷氧基硅烷还有助于固化交联反应的进行，使脱醇型硅有机硅密封胶能顺利固化，使整个体系更加稳定。根据本发明的具体示例，烷基三烷氧基硅烷可以优选为甲基三甲氧基硅烷、乙基三甲氧基硅烷、甲基三乙氧基硅烷和乙基三乙氧基硅烷中的一种或多种，更优选为甲基三甲氧基硅烷。由此可以更有效地防止体系出现粘度下降、黄变等问题，同时可以使脱醇型硅有机硅密封胶能够顺利固化，提高体系稳定性。
在本发明的第二方面，本发明提出了一种脱醇型有机硅密封胶组合物的制备方法。根据本发明的实施例，该方法包括：将前面实施例所述的脱醇型有机硅密封胶组合物含有的成分进行混合。
本发明的方法可以包括将上述组合物含有的成分按照任何形式混合的方法，例如可以采用将上述组合物含有的成分进行一次性混合的方法，或者按照一定的顺序混合的方法。其中，一次性混合的方法可以包括：将烷氧基封端聚二甲基硅氧烷、白炭黑、有机锡催化剂、增塑剂、除水剂、增粘剂和稳定剂进行混合。
根据本发明的实施例，上述混合可以按照下列步骤进行：先在80-150℃的温度下、500-1000rpm的转速下混合300-500min，然后再在15-40℃的温度下、500-1000rpm的转速下混合10-60min。该方法还包括将混合后的产物进行真空脱泡，所述真空脱泡的条件例如可以包括：真空度为-0.1MPa至-0.05MPa、在15-40℃的温度下、500-1000rpm的转速下脱泡8-30min。(转速为搅拌速度)
根据本发明的实施例，优选地，本发明的脱醇型有机硅密封胶的制备方法将按照一定的顺序将上述组合物含有的成分进行混合，即，优选地，上述混合可以按照下列步骤进行：
(1)将烷氧基封端聚二甲基硅氧烷、增塑剂和除水剂进行混合；
(2)将步骤(1)所得的产物与白炭黑进行混合；
(3)将步骤(2)所得的产物与增粘剂进行混合；
(4)将步骤(3)所得的产物、有机锡催化剂和稳定剂进行混合。
根据本发明的实施例，该方法中，所述烷氧基封端聚二甲基硅氧烷、白炭黑、有机锡催化剂、增塑剂、除水剂、增粘剂和稳定剂的种类和用量如上文中所描述的，在此不再赘述。
根据本发明的实施例，优选情况下，步骤(1)的混合条件包括：温度为90-150℃(优选为100-120℃)，时间为30-90min(优选为40-60min)。该混合可以在搅拌速率300-1000rpm(优选为500-900rpm)下进行。该步骤的混合可以达到除水的目的，该混合过程可以通过本领域常规的各种方式进行，例如在动力混合机中进行混合。
根据本发明的实施例，步骤(2)中，白炭黑在混合前优选经过高温烘干，例如在100-150℃下烘干12-30h。优选情况下，步骤(2)的混合条件包括：温度为90-150℃(优选为100-120℃)，时间为30-300min(优选为100-300min)。该混合可以在搅拌速率为600-1500rpm(优选为800-1500rpm)下进行。由此可以进一步提高混合效率和混合均匀度。
根据本发明的具体实施例，更优选地，该方法进一步包括：在进行步骤(2)的混合前，先将步骤(1)所得的产物与白炭黑的混合物进行脱泡处理或者在进行步骤(2) 的混合同时，将步骤(1)所得的产物与白炭黑进行脱泡处理。
根据本发明的具体实施例，在进行步骤(2)的混合前，先将步骤(1)所得的产物与白炭黑进行真空脱泡处理，该真空脱泡处理的条件包括：真空度为-0.1MPa至-0.05MPa，搅拌速度为300-1000rpm(优选为500-900rpm)，温度为80-150℃(优选为90-120℃)，时间为10-60min(优选为20-40min)；或者在进行步骤(2)的混合同时将步骤(1)所得的产物与白炭黑进行真空脱泡处理。优选采用前者，由此可以更加容易操作。
根据本发明的实施例，优选地，步骤(3)的混合条件包括：温度为10-40℃(优选为25-40℃)，时间为10-60min(优选为20-30min)。该混合可以在搅拌速率为300-1000rpm(优选为500-900rpm)下进行。该步骤混合优选在非活泼性气体气氛中进行，例如可以在氮气、氦气和氖气中的一种或多种非活泼性气体的气氛中进行。通过在非活泼性气体气氛中的分散处理，可以有利于缩短以下的真空脱泡处理的时间。
根据本发明的实施例，优选地，步骤(4)的混合条件包括：温度为10-40℃(优选为25-40℃)，时间为10-60min(优选为20-30min)。该混合可以在搅拌速率为300-1000rpm(优选为500-900rpm)下进行。
根据本发明的具体实施例，该方法进一步包括：步骤(5)：将步骤(4)所得的产物进行脱泡处理。具体地，根据本发明的实施例，上述脱泡处理的条件包括：真空度为-0.1MPa至-0.05MPa，搅拌速度为300-1000rpm(优选为500-900rpm)，温度为10-40℃(优选为25-40℃)，时间为10-60min(优选为10-30min)。
当然，需要说明的是，本发明的脱醇型有机硅密封胶并不排除其他的添加剂成分，只要这样的添加剂成分并不影响本发明所得的脱醇型有机硅密封胶的性能即可。作为这样的添加剂例如可以为白矿油。这些添加剂可以在上述任意步骤中加入混合，只要这样的添加不会影响本发明所得的脱醇型有机硅密封胶的性能即可。
以下将通过实施例对本发明进行详细描述。
以下实施例中：
二甲基二氯硅烷表面处理的气相法白炭黑购自EVONIK-DEGUSSA公司AEROSIL R974牌号。
实施例1
本实施例用于说明本发明的脱醇型有机硅密封胶组合物及其制备方法。
(1)将1000g的二甲氧基封端聚二甲基硅氧烷(购自江苏科辛新材料股份公司F-40A牌号，表观粘度为35000mPa·s，以下相同)、200g的甲基硅油(购自广州亚特化工有限公司YT-MS100牌号，表观粘度为100mPa·s，以下相同)和10g的乙烯基三甲氧基硅烷加入到动力混合机中，在120℃下、以900rpm的转速搅拌60min，从而混合除水；
(2)将步骤(1)所得的产物送入真空脱泡机中，并加入200g的二甲基二氯硅烷表面处理的气相法白炭黑(白炭黑已预先在120℃下干燥24h)，并在真空度为-0.06MPa下、120℃下、以900rpm的转速搅拌脱泡30min，而后将产物送入至动力混合机中，常压下、120℃下、以1500rpm的转速搅拌300min；
(3)将步骤(2)所得产物降至室温(约25℃)，并在氮气气氛下加入10g的N-(β-氨乙基)-γ-氨丙基三甲氧基硅烷，并在室温(约25℃)下、以900rpm的转速搅拌20min；
(4)向步骤(3)所得的产物中加入2g的二正丁基二月桂酸锡和30g的甲基三甲氧基硅烷，并在室温(约25℃)下、以900rpm的转速搅拌20min，随后将产物送入至真空脱泡机中，于真空度为-0.06MPa下、30℃下、以900rpm的转速搅拌脱泡10min出料，得到密封胶A1。
实施例2
本实施例用于说明本发明的脱醇型有机硅密封胶组合物及其制备方法。
根据实施例1所述的方法，不同的是，采用180g的甲基硅油，9g的乙烯基三甲氧基硅烷，180g的二甲基二氯硅烷表面处理的气相法白炭黑，9g的N-(β-氨乙基)-γ-氨丙基三甲氧基硅烷，从而得到密封胶A2。
实施例3
本实施例用于说明本发明的脱醇型有机硅密封胶组合物及其制备方法。
根据实施例1所述的方法，不同的是，采用210g的甲基硅油，11g的乙烯基三甲氧基硅烷，210g的二甲基二氯硅烷表面处理的气相法白炭黑，11g的N-(β-氨乙基)-γ-氨丙基三甲氧基硅烷，从而得到密封胶A3。
实施例4
本实施例用于说明本发明的脱醇型有机硅密封胶组合物及其制备方法。
根据实施例1所述的方法，不同的是，采用草酸亚锡代替二正丁基二月桂酸锡，采用三乙氧基封端聚二甲基硅氧烷(购自江苏科辛新材料股份公司E-51牌号，表观粘度为3000mPa·s)替换二甲氧基封端聚二甲基硅氧烷，从而得到密封胶A4。
实施例5
本实施例用于说明本发明的脱醇型有机硅密封胶组合物及其制备方法。
根据实施例1所述的方法，不同的是，N-(β-氨乙基)-γ-氨丙基三甲氧基硅烷的用量为8g，从而得到密封胶A5。
实施例6
本实施例用于说明本发明的脱醇型有机硅密封胶组合物及其制备方法。
根据实施例1所述的方法，不同的是，N-(β-氨乙基)-γ-氨丙基三甲氧基硅烷的用量为12g，从而得到密封胶A6。
实施例7
本实施例用于说明本发明的脱醇型有机硅密封胶组合物及其制备方法。
根据实施例1所述的方法，不同的是，将实施例1采用的全部成分一起在120℃下、以900rpm的转速搅拌410min，再在室温(约25℃)下以900rpm的转速搅拌20min，于真空度为-0.06MPa下、30℃下、以900rpm的转速搅拌脱泡10min出料，得到密封胶A7。
实施例8
本实施例用于说明本发明的脱醇型有机硅密封胶组合物及其制备方法。
根据实施例1所述的方法，不同的是，采用γ-氨丙基三甲氧基硅烷代替N-(β-氨乙基)-γ-氨丙基三甲氧基硅烷，从而制得密封胶A8。
对比例1
根据实施例1所述的方法，不同的是，步骤(4)中不加入甲基三甲氧基硅烷，从而制得密封胶D1。
对比例2
根据实施例1所述的方法，不同的是，采用钛酸丙酯代替二正丁基二月桂酸锡，采用硅烷偶联剂γ-氨丙基三甲氧基硅烷代替N-(β-氨乙基)-γ-氨丙基三甲氧基硅烷，从而制得密封胶D2。
测试例
对上述密封胶A1-A8和D1-D2的表干时间、固化速度、拉伸强度、断裂伸长率、Al-Al粘结强度、透光率、硬度和贮存期进行测量，结果如表1所示，其中：
表干时间的测量方法包括：在(25±5)℃、(55±5)％RH条件下，在干净的聚四氟乙烯板上涂上适量的密封胶，厚度约2mm，每隔1min用手指轻触胶面，至不粘手的时间即为表干时间；
固化速度的测量方法包括：用一个长约300mm，深度为0-10mm渐深的聚四氟乙烯斜槽。向斜槽中挤出适量的密封胶，用刮刀刮平，勿使胶层内有气泡，在(25±2)℃、(55±5)％RH条件下放置24h后从最薄处揭起胶膜，直至未固化的粘连处，测该处槽的深度，以mm/24h表示。
伸强度及断裂伸长率按照GB/T528-1998中记载的方法进行测量；
Al-Al粘结强度是按照GB/T7124-2008中记载的方法进行测量；
透光率按照标准GB/T 2410—2008《透明塑料透光率和雾度的测定》中的规定进行测试，胶片厚度为1mm；
硬度按照GB/T531-1999中记载的方法进行测量；
贮存期的测量方法包括：将装有透明脱醇型密封胶的密封管放入到25℃阴暗干燥的环境中保存，定期(约1个月)取样，挤出观察密封胶的外观状态，并对其力学性能(即伸强度及断裂伸长率)进行测试(按照上述检测实验)，外观状态及性能变化不大的临界时间及为其正常贮存期。
表1
Figure PCTCN2017074623-appb-000001
通过表1的数据可以看出，通过采用本发明的脱醇型有机硅密封胶组合物的成分来制备脱醇型有机硅密封胶时，能够获得兼具较好的弹性和强度的且贮存稳定性较好的脱醇型有机硅密封胶，例如表干时间在20min以下，优选在10min以下，更优选为2-5min；固化速度在4.5mm/24h以上，优选在6-7mm/24h；拉伸强度在1.3MPa以上，优选在1.9MPa以上；断裂伸长率在200％以上，优选在300-380％左右；Al-Al粘结强度在1.2MPa以上，优选在1.7-2MPa；透光率在80％以上，优选在90％以上；硬度邵氏A在15-25；贮存期在3个月以上，优选在6个月以上。
以上详细描述了本发明的优选实施方式，但是，本发明并不限于上述实施方式中的具体细节，在本发明的技术构思范围内，可以对本发明的技术方案进行多种简单变型，这些简单变型均属于本发明的保护范围。
另外需要说明的是，在上述具体实施方式中所描述的各个具体技术特征，在不矛盾的情况下，可以通过任何合适的方式进行组合，为了避免不必要的重复，本发明对各种可能的组合方式不再另行说明。
此外，本发明的各种不同的实施方式之间也可以进行任意组合，只要其不违背本发明的思想，其同样应当视为本发明所公开的内容。

Claims (21)

  1. 一种脱醇型有机硅密封胶组合物，其特征在于，该组合物含有：烷氧基封端聚二甲基硅氧烷、白炭黑、有机锡催化剂、增塑剂、除水剂、增粘剂和稳定剂，其中，所述增塑剂为甲基硅油；所述增粘剂为双氨基硅烷增粘剂、单氨基硅烷增粘剂和烷氧基硅烷增粘剂中的一种或多种；所述稳定剂为烷基三烷氧基硅烷。
  2. 根据权利要求1所述的组合物，其特征在于，相对于100重量份的烷氧基封端聚二甲基硅氧烷，所述白炭黑的用量为5-25重量份，所述有机锡催化剂的用量为0.1-1重量份，所述增塑剂的用量为10-40重量份，所述除水剂的用量为0.5-5重量份，所述增粘剂的用量为0.5-5重量份，所述稳定剂的用量为1-6重量份。
  3. 根据权利要求1或2所述的组合物，其特征在于，相对于100重量份的烷氧基封端聚二甲基硅氧烷，所述白炭黑的用量为10-25重量份，所述有机锡催化剂的用量为0.2-1重量份，所述增塑剂的用量为15-35重量份，所述除水剂的用量为0.5-2重量份，所述增粘剂的用量为0.5-2重量份，所述稳定剂的用量为2-5重量份。
  4. 根据权利要求1-3任一项所述的组合物，其特征在于，所述有机锡催化剂和所述增粘剂的重量比为100：400-600。
  5. 根据权利要求1-4任一项所述的组合物，其特征在于，所述有机锡催化剂和所述增粘剂的重量比为100：450-550。
  6. 根据权利要求1-5任一项所述的组合物，其特征在于，所述有机锡催化剂为二正丁基二月桂酸锡、草酸亚锡和辛酸亚锡中的至少一种。
  7. 根据权利要求6所述的组合物，其特征在于，所述有机锡催化剂为二正丁基二月桂酸锡。
  8. 根据权利要求1-7任一项所述的组合物，其特征在于，所述增塑剂为表观粘度为100-2000mPa·s的甲基硅油。
  9. 根据权利要求1-8任一项所述的组合物，其特征在于，所述除水剂为乙烯基三甲氧基硅烷、无水氯化钙和氧化钙中的一种或多种。
  10. 根据权利要求9所述的组合物，其特征在于，所述除水剂为乙烯基三甲氧基硅烷。
  11. 根据权利要求1-10任一项所述的组合物，其特征在于，所述增粘剂为N-(β-氨乙基)-γ-氨丙基三甲氧基硅烷、γ-氨丙基三甲氧基硅烷和γ-(2,3-环氧丙氧基)丙基三甲氧基硅烷中的至少一种。
  12. 根据权利要求11所述的组合物，其特征在于，所述增粘剂为N-(β-氨乙基)-γ-氨丙基三甲氧基硅烷。
  13. 根据权利要求1-12任一项所述的组合物，其特征在于，所述烷基三烷氧基硅烷为甲基三甲氧基硅烷、乙基三甲氧基硅烷、甲基三乙氧基硅烷和乙基三乙氧基硅烷中的至少一种。
  14. 一种脱醇型有机硅密封胶组合物的制备方法，其特征在于，包括将权利要求1-13任一项所述的组合物含有的成分进行混合。
  15. 根据权利要求14的方法，其特征在于，所述混合按照下列步骤进行：
    (1)将烷氧基封端聚二甲基硅氧烷、增塑剂和除水剂进行混合；
    (2)将步骤(1)所得的产物与白炭黑进行混合；
    (3)将步骤(2)所得的产物与增粘剂进行混合；
    (4)将步骤(3)所得的产物、有机锡催化剂和稳定剂进行混合。
  16. 根据权利要求15所述的方法，其特征在于，步骤(1)的混合是在90-150℃的温度进行30-90min完成的。
  17. 根据权利要求15所述的方法，其特征在于，步骤(2)的混合是在90-150℃的温度进行30-300min完成的。
  18. 根据权利要求15所述的方法，其特征在于，步骤(3)的混合是在10-40℃的温度进行10-60min完成的。
  19. 根据权利要求15所述的方法，其特征在于，步骤(4)的混合是在10-40℃的温度进行10-60min完成的。
  20. 根据权利要求15-19任一项所述的方法，其特征在于，进一步包括：
    在进行步骤(2)的混合前，先将步骤(1)所得的产物与白炭黑的混合物进行脱泡处理；或者
    在进行步骤(2)的混合同时，将步骤(1)所得的产物与白炭黑进行脱泡处理。
  21. 根据权利要求15-20任一项所述的方法，其特征在于，进一步包括：
    (5)将步骤(4)所得的产物进行脱泡处理。
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CN115216268B (zh) * 2022-09-02 2023-08-18 江西蓝星星火有机硅有限公司 脱醇型透明高流动性有机硅密封胶及其制备方法
CN115584238A (zh) * 2022-11-28 2023-01-10 唐山三孚纳米材料有限公司 单组分室温硫化硅橡胶制成的纯白密封胶及其制备方法
CN117757419A (zh) * 2023-12-20 2024-03-26 广东高士高科实业有限公司 一种有机硅断面密封胶及其制备方法
CN117757419B (zh) * 2023-12-20 2024-05-31 广东高士高科实业有限公司 一种有机硅断面密封胶及其制备方法

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