CN110903807A - Preparation method of environment-friendly room temperature vulcanized silicone rubber - Google Patents
Preparation method of environment-friendly room temperature vulcanized silicone rubber Download PDFInfo
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- CN110903807A CN110903807A CN201911180361.8A CN201911180361A CN110903807A CN 110903807 A CN110903807 A CN 110903807A CN 201911180361 A CN201911180361 A CN 201911180361A CN 110903807 A CN110903807 A CN 110903807A
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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
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L83/00—Compositions of 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; Compositions of derivatives of such polymers
- C08L83/04—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
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/24—Acids; Salts thereof
- C08K3/26—Carbonates; Bicarbonates
- C08K2003/265—Calcium, strontium or barium carbonate
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/011—Nanostructured 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
- 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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- 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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- 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
- C08L2205/035—Polymer mixtures characterised by other features containing three or more polymers in a blend containing four or more polymers in a blend
Abstract
The invention relates to a preparation method of environment-friendly single-component room temperature vulcanized silicone rubber, which comprises the following steps of: 30-45 parts of hydroxyl-terminated polydiorganosiloxane, 10-20 parts of a plasticizer, 30-50 parts of a filler, 1-6 parts of pigment and 0.2-1.5 parts of a thixotropic agent are added into a double-planet stirring kettle, stirred and dispersed, 1-5 parts of a water removing agent is added, stirred and dispersed for 30 minutes, 4-8 parts of a cross-linking agent is added, finally 0.2-1 part of a coupling agent and 0.05-0.2 part of a catalyst are added into the kettle, and after uniform mixing, vacuum defoaming and discharging are carried out. The room temperature vulcanized silicone rubber prepared by the invention is a single-component product, is convenient to operate and simple in production process, is nontoxic and environment-friendly, has no corrosivity on metals, electronic components, circuit boards and the like, and has a good bonding effect.
Description
Technical Field
The invention relates to a preparation method of environment-friendly room temperature vulcanized silicone rubber, in particular to a preparation method of environment-friendly room temperature vulcanized silicone rubber without carcinogens in the extrusions during vulcanization.
Background
The single-component room temperature vulcanized silicone rubber has the advantages of convenient construction, room temperature curing, capability of bonding various base materials, excellent weather resistance and the like, and has wide application in various industrial, electronic and building occasions and the like. The single-component room temperature vulcanized silicone rubber can be divided into six types, namely, a deacetylated type, a ketoxime type, a dealcoholized type, a deacetonized type, an amine-removed type and an amide-removed type, according to the type of by-products generated by the crosslinking reaction of a crosslinking agent and hydroxyl-terminated polydiorganosiloxane. The most widely used products in the market at present are deacetylated, ketoxime and dealcoholized products, and the deacetylated products have strong odor irritation and are corrosive to metals; butanone oxime has been identified as a carcinogen in recent years, acetone oxime being in a suspected carcinogen state; methanol released from dealcoholization may cause blindness and the storage stability of the gum is poor.
In order to make up the defects of the existing single-component room temperature vulcanized silicone rubber and protect the environment and the health and safety of human bodies, the patent provides a preparation method of the de-lactylate single-component room temperature vulcanized silicone rubber, and ethyl lactate has the advantages of no toxicity, easy biodegradation and the like.
Disclosure of Invention
The invention provides a preparation method of a demulsified ethyl ester type single-component room temperature vulcanized silicone rubber aiming at the requirement of environmental protection.
A preparation method of environment-friendly single-component room temperature vulcanized silicone rubber comprises the following steps: 30-45 parts of hydroxyl-terminated polydiorganosiloxane, 10-20 parts of plasticizer, 30-50 parts of filler, 1-6 parts of pigment and 0.2-1.5 parts of thixotropic agent are put into a double-planet stirring kettle, the mixture is stirred and dispersed at the speed of 800 rpm at the temperature of 110-150 ℃, the mixture is dehydrated in vacuum for 3-4 hours until the moisture content of the rubber material is less than or equal to 0.05 percent, after the temperature of the rubber material is cooled to 40 ℃, 1-5 parts of water removing agent is added, the mixture is stirred and dispersed for 30 minutes in the vacuum state, 4-8 parts of cross-linking agent is added, the mixture is stirred and dispersed for 20 minutes in the vacuum state, finally 0.2-1 part of coupling agent and 0.05-0.2 part of catalyst are added into the double-planet stirring kettle, the mixture is stirred and dispersed for 20 minutes in the vacuum state, and after the mixture is uniform, the mixture is defoamed in.
On the basis of the technical scheme, the invention can be further improved as follows.
Further, the hydroxyl-terminated polydiorganosiloxane is α, omega-dihydroxy polydimethylsiloxane with the viscosity ranging from 5Pa.s to 20 Pa.s.
Further, the plasticizer is dimethyl silicone oil, and the viscosity range is 100-1000 mPa.s.
Further, the filler is one or a mixture of several of nano calcium carbonate, silicon micropowder and gas-phase silicon dioxide.
The pretreatment of the filler is as follows: uniformly mixing gamma-methacryloxypropyltrimethoxysilane and n-decyltrimethoxysilane according to the molar ratio of 1:1 to prepare an aqueous solution with the concentration of 5.5 percent, and adjusting the pH value of the solution to 8.0; adding a filler into a stirring kettle, uniformly spraying the prepared solution into the filler under the stirring state, stirring for 1.5 hours at room temperature, then heating to 140-150 ℃, vacuumizing, continuously stirring for 8 hours, closing heating, maintaining pressure, cooling to room temperature, discharging, filtering, and drying for later use.
The filler pretreatment can effectively improve the dispersibility of the filler, reduce the moisture content in the filler and is beneficial to the storage stability of the final product (room temperature vulcanized silicone rubber).
Further, the pigment is one of titanium dioxide and carbon black.
Further, the thixotropic agent is one or a mixture of polyether (Pluracol v 10), cyanoethyl trimethoxy silane and bentonite.
Further, the water scavenger is vinyl trimethoxy silane (A-171).
Due to the crosslinking agent employed in the present invention: the activity of the vinyltris (ethyl lactate 2-oxy) silane, the methyltris (ethyl lactate 2-oxy) silane or the tetra (ethyl lactate 2-oxy) silane is relatively low, and a small amount of residual moisture in the system cannot be effectively eliminated, so that the storage stability of the sizing material is poor; the vinyltrimethoxysilane can be used as a moisture scavenger due to the high hydrolysis speed of the vinyltrimethoxysilane, and the addition of the vinyltrimethoxysilane can effectively improve the storage stability of a sealant system.
Further, the cross-linking agent is one or a mixture of more of vinyltris (ethyl lactate 2-oxy) silane, methyltris (ethyl lactate 2-oxy) silane and tetra (ethyl lactate 2-oxy) silane.
Further, the coupling agent is one or a mixture of more of gamma-aminopropyltrimethoxysilane, gamma-glycidoxypropyltrimethoxysilane, N- β -aminoethyl-gamma-aminopropyltrimethoxysilane and gamma-aminopropyltriethoxysilane.
Further, the catalyst is one of dibutyltin dilaurate, stannous octoate, dibutyltin dioctoate and di-n-butyl bis (acetylacetone) tin.
The invention has the beneficial effects that: the room temperature vulcanized silicone rubber prepared by the invention is a single-component product, can be solidified into any shape as required after being contacted with moisture in the air at normal temperature, and is convenient to operate. The production process adopted by the invention is simple, and the prepared room temperature vulcanized silicone rubber is non-toxic and environment-friendly, has no corrosivity on metal, electronic components, circuit boards and the like, and has good bonding effect.
Detailed Description
The following description is made for the purpose of illustrating the principles and features of the present invention and is not intended to limit the scope of the invention.
In the following examples, nano activated calcium carbonate, silica micropowder and fumed silica are all treated fillers.
Example 1
30 parts by mass of α, omega-dihydroxy polydimethylsiloxane with the viscosity of 5Pa.s, 10 parts by mass of simethicone with the viscosity of 100mPa.s, 25 parts by mass of nano calcium carbonate, 5 parts by mass of fumed silica, 1 part by mass of titanium dioxide and 0.2 part by mass of polyether (Pluracol v 10) are put into a double-planet stirring kettle, stirred and dispersed at the speed of 800 rpm at the temperature of 110-150 ℃, dehydrated in vacuum for 3-4 hours until the moisture content of the sizing material is less than or equal to 0.05 percent, after the temperature of the sizing material is cooled to 40 ℃,1 part by mass of vinyl trimethoxy silane is added, stirred and dispersed for 30 minutes in the vacuum state, then 4 parts by mass of vinyl tri (ethyl lactate 2-oxy) silane is added, stirred and dispersed for 20 minutes in the vacuum state, finally 0.2 part by mass of gamma-aminopropyl trimethoxy silane and 0.05 part by mass of di-n-butyl di (acetylacetone) tin are added, stirred and dispersed for 20 minutes in the vacuum state, and after uniform mixing and discharging is carried out.
Example 2
Adding 45 parts by mass of α omega-dihydroxy polydimethylsiloxane with the viscosity of 20Pa.s, 10 parts by mass of simethicone with the viscosity of 1000mPa.s, 40 parts by mass of nano calcium carbonate, 5 parts by mass of fumed silica, 6 parts by mass of titanium dioxide and 1.5 parts by mass of cyanoethyl trimethoxysilane into a double-planet stirring kettle, stirring and dispersing at the speed of 800 rpm at the temperature of 110-150 ℃, dehydrating in vacuum for 3-4 hours until the moisture content of a sizing material is less than or equal to 0.05%, cooling the sizing material to 40 ℃, adding 5 parts by mass of vinyl trimethoxysilane, stirring and dispersing for 30 minutes in the vacuum state, adding 8 parts by mass of vinyl tris (ethyl lactate 2-oxy) silane, stirring and dispersing for 20 minutes in the vacuum state, finally adding 1 part by mass of N- β -aminoethyl-gamma-aminopropyltrimethoxysilane and 0.2 part by mass of dibutyltin dilaurate, continuously stirring and dispersing for 20 minutes in the vacuum state, uniformly mixing, and discharging the product after 30 minutes in vacuum defoaming.
Example 3
Adding 35 parts by mass of α omega-dihydroxy polydimethylsiloxane with the viscosity of 10Pa.s, 15 parts by mass of simethicone with the viscosity of 350mPa.s, 20 parts by mass of silica micropowder, 15 parts by mass of fumed silica, 3 parts by mass of carbon black and 1.0 part by mass of bentonite into a double-planet stirring kettle, stirring and dispersing at the speed of 800 rpm at the temperature of 110-150 ℃, dehydrating in vacuum for 3-4 hours until the moisture content of the sizing material is less than or equal to 0.05%, cooling the sizing material to 40 ℃, adding 3 parts by mass of vinyltrimethoxysilane, stirring and dispersing for 30 minutes in the vacuum state, adding 3 parts by mass of methyltris (ethyl lactate 2-oxy) silane and 3 parts by mass of tetra (ethyl lactate 2-oxy) silane, stirring and dispersing for 20 minutes in the vacuum state, finally adding 0.5 part by mass of gamma-aminopropyltriethoxysilane and 0.1 part by mass of dioctoic acid, continuing stirring and dispersing for 20 minutes in the vacuum state, uniformly mixing, and then discharging for 30 minutes.
Example 4
20 parts by mass of α, omega-dihydroxy polydimethylsiloxane with the viscosity of 5Pa.s, 15 parts by mass of α, omega-dihydroxy polydimethylsiloxane with the viscosity of 20Pa.s, 12 parts by mass of simethicone with the viscosity of 100mPa.s, 10 parts by mass of nano calcium carbonate, 10 parts by mass of silicon micropowder, 10 parts by mass of fumed silica, 3 parts by mass of carbon black and 0.8 part by mass of polyether (Pluracol v 10) are put into a double-planet stirring kettle, stirred and dispersed at the speed of 800 rpm at the temperature of 110-150 ℃, vacuum dehydrated for 3-4 hours until the moisture content of the sizing material is less than or equal to 0.05 percent, after the temperature of the sizing material is cooled to 40 ℃, 2 parts by mass of vinyl trimethoxy silane is added, stirred and dispersed for 30 minutes under a vacuum state, then 4 parts by mass of tetra (ethyl lactate 2-oxy) silane is added, stirred and dispersed for 20 minutes under a vacuum state, finally 0.2 parts by mass of gamma-aminopropyl trimethoxy silane, 0.2 parts by mass of gamma-glycidoxypropyl silane and 0 part by mass of stannous octoate are added, and then uniformly stirred and discharged under a vacuum state, and vacuum defoaming is carried out.
Description of the attached tables
Table 1 shows the comparison of the properties of an environmentally friendly room temperature vulcanized silicone rubber of the present invention.
The properties of an environmentally friendly room temperature vulcanizing silicone rubber of the present invention were tested by the following tests.
Test example 1
Tensile strength: the test was performed according to GB/T528-2009.
Test example 2
Tensile shear strength: the test was carried out according to GB/T7124-2008.
Test example 3
Hardness: the test is carried out according to GB/T531-2008.
Storage stability: viscosity of the oil
The room temperature vulcanized silicone rubber of which the filler is not pretreated or added with vinyltrimethoxysilane is compared with the room temperature vulcanized silicone rubber of examples 1, 2, 3 and 4 for performance test,
the test results were as follows:
from the experimental results in the table, the filler is pretreated before use, and the vinyl trimethoxy silane is used as a water removal agent, so that the prepared de-emulsified ethyl ester type room temperature vulcanized silicone rubber has good storage stability, high tensile strength of the rubber body, good bonding property to a base material, no toxicity, environmental protection and no corrosion to metals such as aluminum, copper and the like.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents, improvements and the like that fall within the spirit and principle of the present invention are intended to be included therein.
Claims (4)
1. The preparation method of the environment-friendly room temperature vulcanized silicone rubber is characterized by comprising the following steps of: putting 30-45 parts of hydroxyl-terminated polydiorganosiloxane, 10-20 parts of a plasticizer, 30-50 parts of a filler, 1-6 parts of a pigment and 0.2-1.5 parts of a thixotropic agent into a double-planet stirring kettle, stirring and dispersing at the speed of 800 rpm at the temperature of 110-150 ℃, dehydrating in vacuum for 3-4 hours until the moisture content of a sizing material is less than or equal to 0.05%, cooling the sizing material to 40 ℃, adding 1-5 parts of a water removing agent, stirring and dispersing for 30 minutes in a vacuum state, then adding 4-8 parts of a cross-linking agent, stirring and dispersing for 20 minutes in the vacuum state, finally adding 0.2-1 part of a coupling agent and 0.05-0.2 part of a catalyst into the double-planet stirring kettle, continuously stirring and dispersing for 20 minutes in the vacuum state, uniformly mixing, and defoaming for 30 minutes in vacuum to discharge;
the pretreatment of the filler is as follows: uniformly mixing gamma-methacryloxypropyltrimethoxysilane and n-decyltrimethoxysilane according to the molar ratio of 1:1 to prepare an aqueous solution with the concentration of 5.5 percent, and adjusting the pH value of the solution to 8.0; adding a filler into a stirring kettle, uniformly spraying the prepared solution into the filler under the stirring state, stirring for 1.5 hours at room temperature, then heating to 140-150 ℃, vacuumizing, continuously stirring for 8 hours, closing heating, maintaining pressure, cooling to room temperature, discharging, filtering, and drying for later use.
2. The method for preparing the environment-friendly room temperature vulcanized silicone rubber according to claim 1, wherein the water scavenger is vinyl trimethoxy silane; the cross-linking agent is one or a mixture of more of vinyl tri (ethyl lactate 2-oxyl) silane, methyl tri (ethyl lactate 2-oxyl) silane and tetra (ethyl lactate 2-oxyl) silane.
3. The preparation method of the environment-friendly room temperature vulcanized silicone rubber according to claim 1, wherein the hydroxyl-terminated polydiorganosiloxane is α, omega-dihydroxy polydimethylsiloxane with the viscosity ranging from 5Pa.s to 20Pa.s, the plasticizer is dimethicone with the viscosity ranging from 100mPa.s to 1000mPa.s, and the filler is one or a mixture of more of nano calcium carbonate, silica micropowder and fumed silica.
4. The method for preparing the environment-friendly room temperature vulcanized silicone rubber according to claim 1, wherein the thixotropic agent is one or a mixture of more of polyether Pluracol v 10, cyanoethyltrimethoxysilane and bentonite, the coupling agent is one or a mixture of more of gamma-aminopropyltrimethoxysilane, gamma-glycidoxypropyltrimethoxysilane, N- β -aminoethyl-gamma-aminopropyltrimethoxysilane and gamma-aminopropyltriethoxysilane, and the catalyst is one of dibutyltin dilaurate, stannous octoate, dibutyltin dioctoate and di-N-butyl bis (acetylacetone) tin.
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2019
- 2019-11-27 CN CN201911180361.8A patent/CN110903807A/en active Pending
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