CN112679958A - Silicon rubber and preparation method thereof, and piezoresistor and preparation method thereof - Google Patents
Silicon rubber and preparation method thereof, and piezoresistor and preparation method thereof Download PDFInfo
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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
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
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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
- C08K7/00—Use of ingredients characterised by shape
- C08K7/22—Expanded, porous or hollow particles
- C08K7/24—Expanded, porous or hollow particles inorganic
- C08K7/26—Silicon- containing compounds
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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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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01C—RESISTORS
- H01C17/00—Apparatus or processes specially adapted for manufacturing resistors
- H01C17/02—Apparatus or processes specially adapted for manufacturing resistors adapted for manufacturing resistors with envelope or housing
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01C—RESISTORS
- H01C7/00—Non-adjustable resistors formed as one or more layers or coatings; Non-adjustable resistors made from powdered conducting material or powdered semi-conducting material with or without insulating material
- H01C7/10—Non-adjustable resistors formed as one or more layers or coatings; Non-adjustable resistors made from powdered conducting material or powdered semi-conducting material with or without insulating material voltage responsive, i.e. varistors
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Abstract
The invention relates to the technical field of materials, in particular to silicon rubber and a preparation method thereof, and a piezoresistor and a preparation method thereof. The silicone rubber is prepared from the following raw materials: the silicon rubber prepared from the formula B hydroxyl-containing vinyl silicone oil, the formula A hydroxyl-containing vinyl silicone oil, a catalyst, white carbon black, a halogen-free environment-friendly flame retardant, aluminum hydroxide, low-hydrogen-containing silicone oil and an inhibitor has good high-temperature and high-humidity resistance and excellent tear resistance.
Description
Technical Field
The invention relates to the technical field of materials, in particular to silicon rubber and a preparation method thereof, and a piezoresistor and a preparation method thereof.
Background
At present, known varistor encapsulation materials mainly include dip-coating type epoxy resin encapsulation powder, dip-coating type liquid epoxy resin, dip-coating type phenolic resin encapsulation powder, dip-coating type organic silicon modified epoxy resin encapsulation powder and dip-coating type self-adhesive liquid addition type silicone rubber. The special-shaped parts such as pins and the like of the piezoresistors prepared by the dip-coating type epoxy resin encapsulation powder, the dip-coating type phenolic resin encapsulation powder and the dip-coating type organic silicon modified epoxy resin encapsulation powder are easy to form stress, the encapsulation material nearby the piezoresistors is easy to crack after being encapsulated, and the encapsulation material is easy to crack after the products are tested by harsh high and low temperature impact (-40 ℃ by 0.5H, 125 ℃ by 0.5H and temperature switching time interval of 3min, 10 cycles and the same below); the pressure-sensitive resistor encapsulated by dip-coated self-adhesive liquid addition type silicon rubber is easy to damage by mechanical force and has uneven thickness due to poor tear resistance of the cured silicon rubber.
The piezoresistor of the dip coating and packaging process has the disadvantages that the bottom is thicker and is 1.0-2.0mm, the corners and the top of the piezoresistor are thinner and are only 0.4-0.8mm, the voltage resistance is unstable, and the breakdown voltage is 5-30 KV.
Disclosure of Invention
The technical problem to be solved by the invention is as follows: a silicon rubber and a preparation method thereof, a piezoresistor and a preparation method thereof are provided.
In order to solve the above technical problems, a first technical solution adopted by the present invention is:
the silicone rubber is prepared from the following raw materials: the flame retardant is composed of B type hydroxyl-containing vinyl silicone oil, A type hydroxyl-containing vinyl silicone oil, a catalyst, white carbon black, a flame retardant, aluminum hydroxide, low-hydrogen-containing silicone oil and an inhibitor.
The second technical scheme adopted by the invention is as follows:
a preparation method of silicone rubber comprises the following steps:
s1, preparing a component A and a component B respectively;
the preparation method of the component A comprises the following steps:
mixing 51-52 parts of B-type hydroxyl-containing vinyl silicone oil, 1.5-3.5 parts of A-type hydroxyl-containing vinyl silicone oil and 0.1-0.3 part of a catalyst to obtain a first mixture;
adding 4-7.5 parts of white carbon black into the first mixture, and mixing to obtain a second mixture;
sequentially adding 12.5-17.5 parts of flame retardant and 17.5-22.5 parts of aluminum hydroxide into the second mixture, and mixing to obtain a component A;
the preparation method of the component B comprises the following steps:
mixing 48-49 parts of B-type hydroxyl-containing vinyl silicone oil, 1.5-3.5 parts of A-type hydroxyl-containing vinyl silicone oil, 8-12 parts of low-hydrogen-containing silicone oil and 0.1-0.3 part of inhibitor to obtain a third mixture;
adding 4-7.5 parts of white carbon black into the third mixture, and mixing to obtain a fourth mixture;
sequentially adding 12.5-17.5 parts of flame retardant and 17.5-22.5 parts of aluminum hydroxide into the fourth mixture, and mixing to obtain a component B;
and S2, mixing the component A and the component B to obtain the silicone rubber.
The third technical scheme adopted by the invention is as follows:
the packaging material of the piezoresistor is the silicon rubber.
The fourth technical scheme adopted by the invention is as follows:
a preparation method of a piezoresistor comprises the following steps:
placing a piezoresistor to be processed in a mould;
and injecting the silicon rubber into the mold, closing the silicon rubber and the piezoresistor to be processed, and demolding after molding to obtain the piezoresistor.
The invention has the beneficial effects that:
the invention provides silicon rubber and a preparation method thereof, and a piezoresistor and a preparation method thereof, wherein the liquid silicon rubber is prepared from the following raw materials: the silicon rubber prepared from the formula B hydroxyl-containing vinyl silicone oil, the formula A hydroxyl-containing vinyl silicone oil, a catalyst, white carbon black, a flame retardant, aluminum hydroxide, low-hydrogen-containing silicone oil and an inhibitor has good high-temperature and high-humidity resistance and excellent tear resistance. And the silicone rubber is prepared by the preparation method. The silicon rubber is applied to the piezoresistor as an encapsulating material of the piezoresistor and organically combined with the piezoresistor, meanwhile, in the preparation process of the piezoresistor, after the silicon rubber is subjected to injection molding, the thickness of the silicon rubber can be controlled through a mold, and the surface of the silicon rubber is smooth.
Detailed Description
In order to explain the technical content, the objects and the effects of the present invention in detail, the following description will be given with reference to the embodiments.
The invention provides silicon rubber which is prepared from the following raw materials: the flame retardant is composed of B type hydroxyl-containing vinyl silicone oil, A type hydroxyl-containing vinyl silicone oil, a catalyst, white carbon black, a flame retardant, aluminum hydroxide, low-hydrogen-containing silicone oil and an inhibitor.
From the above description, the beneficial effects of the present invention are:
the silicone rubber is prepared from the following raw materials: the silicon rubber prepared from the formula B hydroxyl-containing vinyl silicone oil, the formula A hydroxyl-containing vinyl silicone oil, a catalyst, white carbon black, a flame retardant, aluminum hydroxide, low-hydrogen-containing silicone oil and an inhibitor has good high-temperature and high-humidity resistance and excellent tear resistance. The viscosity of the silicon rubber provided by the invention before curing is 70-90 Pa.s, and the density is 1.1-1.3g/cm3Performance of the silicone rubber after curing: the tensile strength can reach 6-9MPa, the elongation at break can reach 350-500%, the tear strength (right angle) is more than or equal to 16kN/m, the Shore hardness A is 30-60, the electrical strength is more than or equal to 20kV/mm, and the dielectric loss is (50Hz)1 (+/-0.2) multiplied by 10-4The dielectric constant was (50Hz)2.5 (+ -0.2), the tracking resistance was 1A4.5, and the flame retardance was FV0/1 mm.
Wherein, the high temperature and high humidity resistance is shown in the following: for example, the voltage dependent resistor of 621V, the encapsulated product, after the temperature is 85 ℃, the humidity is 85%, the loaded direct current voltage is 500Vd, the voltage dependent voltage change rate is less than 10% after 1000h test, and the leakage current is less than 25 muA;
the excellent tear resistance is shown in the following: 0.5h at-40 ℃ and 0.5h at 125 ℃ with a temperature switching time interval of 3min, no cracking after 20 cycles.
Further, the food is prepared from the following raw materials in parts by weight: 95-105 parts of B-type hydroxyl-containing vinyl silicone oil, 3-7 parts of A-type hydroxyl-containing vinyl silicone oil, 0.1-0.3 part of catalyst, 8-15 parts of white carbon black, 25-35 parts of flame retardant, 35-45 parts of aluminum hydroxide, 8-12 parts of low-hydrogen-containing silicone oil and 0.1-0.3 part of inhibitor.
Wherein, 8 to 15 parts of white carbon black, the corresponding product is injection type silicon rubber, and if 15 to 25 parts of white carbon black, the corresponding product is mould pressing type silicon rubber.
Further, the food is prepared from the following raw materials in parts by weight: 100 parts of B-type hydroxyl-containing vinyl silicone oil, 5 parts of A-type hydroxyl-containing vinyl silicone oil, 0.2 part of catalyst, 10 parts of white carbon black, 30 parts of flame retardant, 40 parts of aluminum hydroxide, 10 parts of low-hydrogen-containing silicone oil and 0.2 part of inhibitor.
Furthermore, the color paste is also included. The color paste plays the roles of color mixing and thixotropy increasing. 1.5 parts of color paste according to the mixture ratio.
Further, the adhesive also comprises a tackifier.
Further, the weight ratio of the tackifier to the catalyst is 1:1, the viscosity of the B-type hydroxyl-containing vinyl silicone oil is 30 Pa.s, the viscosity of the low-hydrogen-containing silicone oil is 300-500mPa.s, and the active hydrogen content of the low-hydrogen-containing silicone oil is 0.35-0.50%.
Further, the viscosity of the hydroxyl-containing vinyl silicone oil in the formula B is 40Pa.s, and the viscosity of the low-hydrogen silicone oil is more than 300 mPa.s.
The invention provides a preparation method of silicone rubber, which comprises the following steps:
s1, preparing a component A and a component B respectively;
the preparation method of the component A comprises the following steps:
mixing 51-52 parts of B-type hydroxyl-containing vinyl silicone oil, 1.5-3.5 parts of A-type hydroxyl-containing vinyl silicone oil and 0.1-0.3 part of a catalyst to obtain a first mixture;
adding 4-7.5 parts of white carbon black into the first mixture, and mixing to obtain a second mixture;
sequentially adding 12.5-17.5 parts of flame retardant and 17.5-22.5 parts of aluminum hydroxide into the second mixture, and mixing to obtain a component A;
the preparation method of the component B comprises the following steps:
mixing 48-49 parts of B-type hydroxyl-containing vinyl silicone oil, 1.5-3.5 parts of A-type hydroxyl-containing vinyl silicone oil, 8-12 parts of low-hydrogen-containing silicone oil and 0.1-0.3 part of inhibitor to obtain a third mixture;
adding 4-7.5 parts of white carbon black into the third mixture, and mixing to obtain a fourth mixture;
sequentially adding 12.5-17.5 parts of flame retardant and 17.5-22.5 parts of aluminum hydroxide into the fourth mixture, and mixing to obtain a component B;
and S2, mixing the component A and the component B to obtain the silicone rubber.
From the above description, the beneficial effects of the present invention are: the silicone rubber is prepared by the above preparation method.
Further, the preparation method of the component A specifically comprises the following steps:
mixing 51.9 parts of the hydroxyl-containing vinyl silicone oil of the formula B, 2.5 parts of the hydroxyl-containing vinyl silicone oil of the formula A and 0.2 part of a catalyst to obtain a first mixture;
adding 5 parts of white carbon black into the first mixture, and mixing to obtain a second mixture;
sequentially adding 15 parts of flame retardant and 20 parts of aluminum hydroxide into the second mixture, and mixing to obtain a component A;
the preparation method of the component B comprises the following specific steps:
mixing 48.1 parts of the hydroxyl-containing vinyl silicone oil of the formula B, 2.5 parts of the hydroxyl-containing vinyl silicone oil of the formula A, 10 parts of low-hydrogen-containing silicone oil and 0.2 part of an inhibitor to obtain a third mixture;
adding 5 parts of white carbon black into the third mixture, and mixing to obtain a fourth mixture;
and adding 15 parts of flame retardant and 20 parts of aluminum hydroxide into the fourth mixture in sequence, and mixing to obtain a component B.
Further, the preparation method of the component A specifically comprises the following steps:
mixing 51.9 parts of a B-type hydroxyl-containing vinyl silicone oil with the viscosity of 30 pas, 2.5 parts of an A-type hydroxyl-containing vinyl silicone oil, 0.2 part of a catalyst and 0.2 part of a tackifier to obtain a first mixture;
adding 5 parts of white carbon black into the first mixture, and mixing to obtain a second mixture;
sequentially adding 15 parts of flame retardant and 20 parts of aluminum hydroxide into the second mixture, and mixing to obtain a component A;
the preparation method of the component B comprises the following specific steps:
mixing 48.1 parts of a hydroxyl-containing vinyl silicone oil of formula B having a viscosity of 30 pas, 2.5 parts of a hydroxyl-containing vinyl silicone oil of formula A, 10 parts of a low-hydrogen-containing silicone oil having a high viscosity, and 0.2 part of an inhibitor to obtain a third mixture;
adding 5 parts of white carbon black into the third mixture, and mixing to obtain a fourth mixture;
and adding 15 parts of flame retardant and 20 parts of aluminum hydroxide into the fourth mixture in sequence, and mixing to obtain a component B.
The tackifier is applied to the surface of a metal base material, the surface of an inorganic base material and the surface of an organic material, can effectively improve the surface performance of the base material and increase the adhesion between the base material and the adhesive. The chemical reaction between the hydroxyl group on the surface of the substrate and the active hydrogen, hydroxyl group and the like of the silicon rubber respectively forms a firm chemical bond (covalent bond) on two interfaces, and the chemical bond on the interface has higher bonding strength because the bond energy of the chemical bond is larger than the acting force between molecules.
Further, the preparation method of the component B specifically comprises the following steps:
mixing 48-49 parts of B-type hydroxyl-containing vinyl silicone oil, 1.5-3.5 parts of A-type hydroxyl-containing vinyl silicone oil, 8-12 parts of low-hydrogen-containing silicone oil and 0.1-0.3 part of inhibitor to obtain a third mixture;
adding 4-7.5 parts of white carbon black into the third mixture, and mixing to obtain a fourth mixture;
and sequentially adding 12.5-17.5 parts of flame retardant, 1-2 parts of color paste and 17.5-22.5 parts of aluminum hydroxide into the fourth mixture, and mixing to obtain a component B.
The packaging material of the piezoresistor is the silicon rubber.
The invention also provides a preparation method of the piezoresistor, which comprises the following steps:
placing a piezoresistor to be processed in a mould;
and injecting the silicon rubber into the mold, closing the silicon rubber and the piezoresistor to be processed, and demolding after molding to obtain the piezoresistor.
From the above description, the beneficial effects of the present invention are: the silicon rubber is applied to the piezoresistor as an encapsulating material of the piezoresistor and organically combined with the piezoresistor, meanwhile, in the preparation process of the piezoresistor, after the silicon rubber is subjected to injection molding, the thickness of the silicon rubber can be controlled through a mold, the surface of the silicon rubber is smooth, compared with other encapsulating materials of dip-coating type, the problem of sagging (uneven surface) caused by the action of gravity after dip-coating can be solved, the silicon rubber has good binding force with each part of the piezoresistor and belongs to chemical bonding property, xylene or other solvents are not volatilized in the curing process, and the cured silicon rubber is not easy to strip.
The first embodiment of the invention is as follows:
the liquid silicone rubber is prepared from the following raw materials: the flame retardant is composed of B type hydroxyl-containing vinyl silicone oil, A type hydroxyl-containing vinyl silicone oil, a catalyst, white carbon black, a flame retardant, aluminum hydroxide, low-hydrogen-containing silicone oil and an inhibitor.
Wherein, the viscosity of the B-type hydroxyl-containing vinyl silicone oil is 30-50 Pa.s; the viscosity of the hydroxyl-containing vinyl silicone oil of the formula A is more than 4000 mPa.s;
the catalyst is Karstedt platinum catalyst or peroxide type vulcanizing agent (such as 2, 5-dimethyl-2, 5-di (tert-butylperoxy) hexane);
the specific surface area of the white carbon black is 140-250m2And/g, the white carbon black is less than 15 percent (preferably 8-15 parts) of the B-type hydroxyl vinyl silicone oil, the silicone rubber is easy to be in a liquid state and is suitable for an injection process, and the white carbon black is more than 15 percent, the silicone rubber is easy to be in a solid state and is suitable for a compression molding process.
The active hydrogen content of the low-hydrogen silicone oil is 0.35-0.5%. In this example, the white carbon black had been treated with hexamethyldisilazane; the flame retardant is a halogen-free environment-friendly flame retardant containing nitrogen, phosphorus, silicon elements and benzene rings (P, N exists in the form of a high molecular organic compound, and a platinum catalytic system is not poisoned); the inhibitor is a mixed solution of methylbutynol and 1-ethynyl cyclohexanol.
The structural formula of the A-type hydroxyl-containing vinyl silicone oil is as follows:
the structural formula of the B type hydroxyl-containing vinyl silicone oil is as follows:
the structural formula of the low hydrogen-containing silicone oil is as follows:
the second embodiment of the invention is as follows:
the silicone rubber is prepared from the following raw materials in parts by weight: 95-105 parts of B-type hydroxyl-containing vinyl silicone oil, 3-7 parts of A-type hydroxyl-containing vinyl silicone oil, 0.1-0.3 part of catalyst, 8-15 parts of white carbon black, 25-35 parts of flame retardant, 35-45 parts of aluminum hydroxide, 8-12 parts of low-hydrogen-containing silicone oil and 0.1-0.3 part of inhibitor.
The third embodiment of the invention is as follows:
the silicone rubber is prepared from the following raw materials in parts by weight: 95 parts of B-type hydroxyl-containing vinyl silicone oil, 3 parts of A-type hydroxyl-containing vinyl silicone oil, 0.1 part of catalyst, 8 parts of white carbon black, 25 parts of flame retardant, 35 parts of aluminum hydroxide, 8 parts of low-hydrogen-containing silicone oil and 0.1 part of inhibitor.
The fourth embodiment of the invention is as follows:
the silicone rubber is prepared from the following raw materials in parts by weight: 100 parts of B-type hydroxyl-containing vinyl silicone oil, 5 parts of A-type hydroxyl-containing vinyl silicone oil, 0.2 part of catalyst, 10 parts of white carbon black, 30 parts of flame retardant, 40 parts of aluminum hydroxide, 10 parts of low-hydrogen-containing silicone oil and 0.2 part of inhibitor.
The fifth embodiment of the invention is as follows:
the silicone rubber is prepared from the following raw materials in parts by weight: 105 parts of B-type hydroxyl-containing vinyl silicone oil, 7 parts of A-type hydroxyl-containing vinyl silicone oil, 0.3 part of platinum catalyst, 15 parts of white carbon black, 35 parts of flame retardant, 45 parts of aluminum hydroxide, 12 parts of low-hydrogen-containing silicone oil, 0.3 part of inhibitor and 2 parts of color paste.
The sixth embodiment of the invention is as follows:
on the basis of the first embodiment, the raw material of the silicone rubber also comprises a tackifier.
The seventh embodiment of the invention is:
on the basis of the sixth embodiment, the following features are further defined: the weight ratio of the tackifier to the catalyst is 1:1, the viscosity of the B-type hydroxyl-containing vinyl silicone oil is 30 Pa.s, the viscosity of the low-hydrogen-containing silicone oil is 300-500mPa.s, and the active hydrogen content of the low-hydrogen-containing silicone oil is 0.35-0.50%.
The eighth embodiment of the present invention is:
on the basis of the first embodiment, the following features are further defined: the viscosity of the B-type hydroxyl-containing vinyl silicone oil is 40Pa.s, and the viscosity of the low-hydrogen-containing silicone oil is more than 300 mPa.s.
The ninth embodiment of the invention is:
the invention provides a preparation method of silicone rubber, which comprises the following steps:
s1, preparing a component A and a component B respectively;
the preparation method of the component A comprises the following steps:
mixing 51-52 parts of B-type hydroxyl-containing vinyl silicone oil, 1.5-3.5 parts of A-type hydroxyl-containing vinyl silicone oil and 0.1-0.3 part of a catalyst to obtain a first mixture;
adding 4-7.5 parts of white carbon black into the first mixture, and mixing to obtain a second mixture;
sequentially adding 12.5-17.5 parts of flame retardant and 17.5-22.5 parts of aluminum hydroxide into the second mixture, and mixing to obtain a component A;
the preparation method of the component B comprises the following steps:
mixing 48-49 parts of B-type hydroxyl-containing vinyl silicone oil, 1.5-3.5 parts of A-type hydroxyl-containing vinyl silicone oil, 8-12 parts of low-hydrogen-containing silicone oil and 0.1-0.3 part of inhibitor to obtain a third mixture;
adding 4-7.5 parts of white carbon black into the third mixture, and mixing to obtain a fourth mixture;
sequentially adding 12.5-17.5 parts of flame retardant and 17.5-22.5 parts of aluminum hydroxide into the fourth mixture, and mixing to obtain a component B;
and S2, mixing the component A and the component B to obtain the silicone rubber.
The tenth embodiment of the present invention is:
the invention provides a preparation method of silicone rubber, which comprises the following steps:
s1, preparing a component A and a component B respectively;
the preparation method of the component A comprises the following steps:
mixing 51 parts of B-type hydroxyl-containing vinyl silicone oil, 1.5 parts of A-type hydroxyl-containing vinyl silicone oil and 0.1 part of catalyst to obtain a first mixture;
adding 4 parts of white carbon black into the first mixture, and mixing to obtain a second mixture;
adding 12.5 parts of flame retardant and 17.5 parts of aluminum hydroxide into the second mixture in sequence, and mixing to obtain a component A;
the preparation method of the component B comprises the following steps:
mixing 48 parts of B-type hydroxyl-containing vinyl silicone oil, 1.5 parts of A-type hydroxyl-containing vinyl silicone oil, 8 parts of low-hydrogen-containing silicone oil and 0.1 part of inhibitor to obtain a third mixture;
adding 4 parts of white carbon black into the third mixture, and mixing to obtain a fourth mixture;
adding 12.5 parts of flame retardant, 1 part of color paste and 17.5 parts of aluminum hydroxide into the fourth mixture in sequence, and mixing to obtain a component B;
and S2, mixing the component A and the component B to obtain the silicone rubber.
The eleventh embodiment of the present invention is:
the invention provides a preparation method of silicone rubber, which comprises the following steps:
s1, preparing a component A and a component B respectively;
the preparation method of the component A comprises the following steps:
mixing 52 parts of B-type hydroxyl-containing vinyl silicone oil, 3.5 parts of A-type hydroxyl-containing vinyl silicone oil and 0.3 part of catalyst to obtain a first mixture;
adding 7.5 parts of white carbon black into the first mixture, and mixing to obtain a second mixture;
adding 17.5 parts of flame retardant and 22.5 parts of aluminum hydroxide into the second mixture in sequence, and mixing to obtain a component A;
the preparation method of the component B comprises the following steps:
mixing 49 parts of B-type hydroxyl-containing vinyl silicone oil, 3.5 parts of A-type hydroxyl-containing vinyl silicone oil, 12 parts of low-hydrogen-containing silicone oil and 0.3 part of inhibitor to obtain a third mixture;
adding 7.5 parts of white carbon black into the third mixture, and mixing to obtain a fourth mixture;
adding 17.5 parts of flame retardant and 22.5 parts of aluminum hydroxide into the fourth mixture in sequence, and mixing to obtain a component B;
and S2, mixing the component A and the component B to obtain the silicone rubber.
The twelfth embodiment of the present invention is:
the invention provides a preparation method of silicone rubber, which comprises the following steps:
s1, preparing a component A and a component B respectively;
the preparation method of the component A comprises the following specific steps:
mixing 51.9 parts of the hydroxyl-containing vinyl silicone oil of the formula B, 2.5 parts of the hydroxyl-containing vinyl silicone oil of the formula A and 0.2 part of a catalyst to obtain a first mixture;
adding 5 parts of white carbon black into the first mixture, and mixing to obtain a second mixture;
sequentially adding 15 parts of flame retardant and 20 parts of aluminum hydroxide into the second mixture, and mixing to obtain a component A;
the preparation method of the component B comprises the following specific steps:
mixing 48.1 parts of the hydroxyl-containing vinyl silicone oil of the formula B, 2.5 parts of the hydroxyl-containing vinyl silicone oil of the formula A, 10 parts of low-hydrogen-containing silicone oil and 0.2 part of an inhibitor to obtain a third mixture;
adding 5 parts of white carbon black into the third mixture, and mixing to obtain a fourth mixture;
sequentially adding 15 parts of flame retardant and 20 parts of aluminum hydroxide into the fourth mixture, and mixing to obtain a component B;
and S2, mixing the component A and the component B to obtain the silicone rubber.
The twelfth embodiment of the present invention is:
in addition to the above-mentioned example eleven, there is further defined a feature that the viscosity of the hydroxyl group-containing vinyl silicone oil of the formula B in both the A component and the B component is 20 pas. The silicone rubber prepared by this example had a viscosity of 70 pas before curing and a density of 1.3g/cm3Properties after curing: the tensile strength is 6MPa, the elongation at break is 350 percent, the tear strength (right angle) is 16kN/m, the electrical strength is 22kV/mm, and the dielectric loss is (50Hz)1.1 multiplied by 10-4The dielectric constant was (50Hz)2.5, the tracking resistance was 1A4.5, and the flame retardance was FV0/1 mm. GB/T7124, the shear strength of the tin-coated copper-VS-tin-coated copper or the copper-VS-copper is 1.1 MPa. The Shore A hardness after curing was 60.
The embodiment is implemented specifically as follows:
preparation of component A:
adding 51.9kg of B-type hydroxyl-containing vinyl silicone oil with the viscosity of 20 Pa.s into the reaction kettle, then adding 2.5kg of A-type hydroxyl-containing vinyl silicone oil and 0.2kg of platinum catalyst, and fully and uniformly stirring;
then adding 5kg of white carbon black treated by hexamethyldisilazane for several times, and fully and uniformly stirring;
15kg of halogen-free environment-friendly flame retardant (P, N exists in the form of a high molecular organic compound, and a platinum catalytic system is not poisoned) containing nitrogen, phosphorus, silicon elements and benzene rings is added;
adding 20kg of aluminum hydroxide filler, stirring uniformly and defoaming.
Preparation of the component B:
adding 48.1kg of the hydroxyl-containing vinyl silicone oil of the formula B with the viscosity of 20 Pa.s into a reaction kettle, then adding 2.5kg of the hydroxyl-containing vinyl silicone oil of the formula A, 10kg of low-hydrogen silicone oil and 0.2kg of an inhibitor (a mixed solution of methylbutynol and 1-ethynyl cyclohexanol), and fully and uniformly stirring;
then adding 5kg of white carbon black treated by hexamethyldisilazane for several times, and fully and uniformly stirring;
15kg of halogen-free environment-friendly flame retardant containing nitrogen, phosphorus, silicon elements and benzene rings is added;
adding 1.5kg of color paste;
adding 20kg of aluminum hydroxide filler, stirring uniformly and defoaming.
The thirteenth embodiment of the present invention is:
the invention provides a preparation method of silicone rubber, which comprises the following steps:
s1, preparing a component A and a component B respectively;
the preparation method of the component A comprises the following specific steps:
mixing 51.9 parts of B-type hydroxyl-containing vinyl silicone oil with the viscosity of 30 Pa.s, 2.5 parts of A-type hydroxyl-containing vinyl silicone oil, 0.2 part of platinum catalyst and 0.2 part of tackifier to obtain a first mixture;
adding 5 parts of white carbon black into the first mixture, and mixing to obtain a second mixture;
sequentially adding 15 parts of halogen-free environment-friendly flame retardant and 20 parts of aluminum hydroxide into the second mixture, and mixing to obtain a component A;
the preparation method of the component B comprises the following specific steps:
mixing 48.1 parts of a hydroxyl-containing vinyl silicone oil of formula B having a viscosity of 30 pas, 2.5 parts of a hydroxyl-containing vinyl silicone oil of formula A, 10 parts of a low-hydrogen-containing silicone oil having a high viscosity, and 0.2 part of an inhibitor to obtain a third mixture;
adding 5 parts of white carbon black into the third mixture, and mixing to obtain a fourth mixture;
and sequentially adding 15 parts of halogen-free environment-friendly flame retardant, 1.5 parts of color paste and 20 parts of aluminum hydroxide into the fourth mixture, and mixing to obtain a component B.
And S2, mixing the component A and the component B to obtain the silicone rubber.
The silicone rubber prepared by this example was,viscosity before curing was 85 pas and density was 1.2g/cm3Properties after curing: tensile strength of 7.2MPa, elongation at break of 500%, tear strength (right angle) of 22kN/m, electrical strength of 23kV/mm, dielectric loss of (50Hz)1.2) x 10-4The dielectric constant was (50Hz)2.7, the tracking resistance was 1A4.5, and the flame retardance was FV0/1 mm. GB/T7124, the shear strength of the tin-coated copper-VS-tin-coated copper or the copper-VS-copper is 1.2 MPa. The Shore A hardness after curing was 45.
The embodiment is implemented specifically as follows:
preparation of component A:
adding 51.9kg of B-type hydroxyl-containing vinyl silicone oil with the viscosity of 30 Pa.s into the reaction kettle, then adding 2.5kg of A-type hydroxyl-containing vinyl silicone oil, 0.2kg of platinum catalyst and 0.2kg of tackifier containing epoxy groups, and fully and uniformly stirring;
then adding 5kg of white carbon black treated by hexamethyldisilazane for several times, and fully and uniformly stirring;
15kg of halogen-free environment-friendly flame retardant containing nitrogen, phosphorus, silicon elements and benzene rings is added;
adding 20kg of aluminum hydroxide filler, stirring uniformly and defoaming.
Preparation of the component B:
adding 48.1kg of the hydroxyl-containing vinyl silicone oil of the formula B with the viscosity of 30 Pa.s into a reaction kettle, adding 2.5kg of the hydroxyl-containing vinyl silicone oil of the formula A and 10kg of low-hydrogen silicone oil with high viscosity (the viscosity of the low-hydrogen silicone oil is more than 300mPa.s), and 0.2kg of an inhibitor (a mixed solution of methyl butynol and 1-ethynyl cyclohexanol), and fully and uniformly stirring;
then adding 5kg of white carbon black treated by hexamethyldisilazane for several times, and fully and uniformly stirring;
15kg of halogen-free environment-friendly flame retardant containing nitrogen, phosphorus, silicon elements and benzene rings is added;
adding 1.5kg of color paste;
adding 20kg of aluminum hydroxide filler, stirring uniformly and defoaming.
The fourteenth embodiment of the present invention is:
in addition to the above-mentioned example eleven, there is further defined a feature that the viscosity of the hydroxyl group-containing vinyl silicone oil of the formula B in both the a component and the B component is 40Pa · s, and the low hydrogen-containing silicone oil is a high-viscosity low hydrogen-containing silicone oil. The silicone rubber prepared by this example had a viscosity of 90 pas before curing and a density of 1.3g/cm3Properties after curing: the tensile strength can reach 7MPa, the elongation at break can reach 450 percent, the tear strength (right angle) is 18kN/m, the electrical strength is more than or equal to 21kV/mm, and the dielectric loss is (50Hz)1.0 multiplied by 10-4The dielectric constant was (50Hz)2.5, the tracking resistance was 1A4.5, and the flame retardance was FV0/1 mm. GB/T7124, the shear strength of the tin-coated copper-VS-tin-coated copper or the copper-VS-copper is 1.0 MPa. The Shore A hardness after curing was 30.
The embodiment is implemented specifically as follows:
preparation of component A:
adding 51.9kg of B-type hydroxyl-containing vinyl silicone oil with the viscosity of 40Pa.s into the reaction kettle, then adding 2.5kg of A-type hydroxyl-containing vinyl silicone oil and 0.2kg of platinum catalyst, and fully and uniformly stirring;
then adding 5kg of white carbon black treated by hexamethyldisilazane for several times, and fully and uniformly stirring;
15kg of halogen-free environment-friendly flame retardant (P, N exists in the form of a high molecular organic compound, and a platinum catalytic system is not poisoned) containing nitrogen, phosphorus, silicon elements and benzene rings is added;
adding 20kg of aluminum hydroxide filler, stirring uniformly and defoaming.
Preparation of the component B:
adding 48.1kg of the hydroxyl-containing vinyl silicone oil of the formula B with the viscosity of 40Pa.s into a reaction kettle, adding 2.5kg of the hydroxyl-containing vinyl silicone oil of the formula A and 10kg of low-hydrogen silicone oil with high viscosity (the viscosity of the low-hydrogen silicone oil is more than 300mPa.s), and 0.2kg of an inhibitor (a mixed solution of methyl butynol and 1-ethynyl cyclohexanol), and fully and uniformly stirring;
then adding 5kg of white carbon black treated by hexamethyldisilazane for several times, and fully and uniformly stirring;
15kg of halogen-free environment-friendly flame retardant containing nitrogen, phosphorus, silicon elements and benzene rings is added;
adding 1.5kg of color paste;
adding 20kg of aluminum hydroxide filler, stirring uniformly and defoaming.
Fifteenth embodiment of the present invention is:
the packaging material of the piezoresistor is the silicon rubber.
The sixteenth embodiment of the present invention is:
a preparation method of a piezoresistor comprises the following steps:
placing a piezoresistor to be processed in a mould;
and injecting the silicon rubber into the mold, closing the silicon rubber and the piezoresistor to be processed, and demolding after molding to obtain the piezoresistor.
Wherein the injection operation is performed by an injection molding machine. In order to better avoid the generation of waste rubber edges and reduce the difference degree of internal stress of each part after injection molding, a vertical injection molding machine is selected. The equipment parameters of the vertical injection molding machine are as follows in table 1.
TABLE 1
The component A of the barrel A, the component B of the barrel B and the color paste of the barrel P are metered by a feeding device through a proportioning valve, conveyed to a premixing chamber, mixed by a static shunting mixer and injected into a mold, after mold closing, the injection type silicon rubber is spread on components and parts and is heated and cured, according to the difference of sample sizes, no redundant rubber edge is generated, and the process parameters can refer to the following table 2:
TABLE 2
In order to facilitate the product to be demoulded from the mould, a self-lubricating coating or a polytetrafluoroethylene coating with the thickness of 5 microns can be sprayed on the interior of the mould in advance, and the self-lubricating coating or the polytetrafluoroethylene coating is baked and cured at 150 ℃ for 10min and 380 ℃ for 10 min.
In summary, the silicone rubber and the preparation method thereof, and the piezoresistor and the preparation method thereof provided by the invention are provided, wherein the silicone rubber is prepared from the following raw materials: the liquid silicone rubber has the advantages that the liquid silicone rubber has good high-temperature and high-humidity resistance and excellent tear resistance. And the silicone rubber is prepared by the preparation method. The silicon rubber is applied to the piezoresistor as an encapsulating material of the piezoresistor and organically combined with the piezoresistor, meanwhile, in the preparation process of the piezoresistor, after the silicon rubber is subjected to injection molding, the thickness of the silicon rubber can be controlled through a mold, and the surface of the silicon rubber is smooth.
The above description is only an embodiment of the present invention, and not intended to limit the scope of the present invention, and all equivalent modifications made by the present invention in the specification or directly or indirectly applied to the related technical field are included in the scope of the present invention.
Claims (12)
1. The silicon rubber is characterized by comprising the following raw materials: the flame retardant is composed of B type hydroxyl-containing vinyl silicone oil, A type hydroxyl-containing vinyl silicone oil, a catalyst, white carbon black, a flame retardant, aluminum hydroxide, low-hydrogen-containing silicone oil and an inhibitor.
2. The silicone rubber according to claim 1, which is prepared from the following raw materials in parts by weight: 95-105 parts of B-type hydroxyl-containing vinyl silicone oil, 3-7 parts of A-type hydroxyl-containing vinyl silicone oil, 0.1-0.3 part of catalyst, 8-15 parts of white carbon black, 25-35 parts of flame retardant, 35-45 parts of aluminum hydroxide, 8-12 parts of low-hydrogen-containing silicone oil and 0.1-0.3 part of inhibitor.
3. The silicone rubber according to claim 2, further comprising a color paste.
4. A silicone rubber according to any one of claims 1-3, further comprising a tackifier.
5. The silicone rubber according to claim 4, wherein the weight ratio of the tackifier to the catalyst is 1:1, the viscosity of the B-type hydroxyl-containing vinyl silicone oil is 30 Pa-s, the viscosity of the low hydrogen-containing silicone oil is 300-500mPa.s, and the active hydrogen content of the low hydrogen-containing silicone oil is 0.35-0.50%.
6. The silicone rubber according to claim 1, wherein the viscosity of the hydroxyl-containing vinyl silicone oil of formula B is 40Pa.s, and the viscosity of the low hydrogen-containing silicone oil is more than 300 mPa.s.
7. A method for preparing the silicone rubber of claim 1, comprising the steps of:
s1, preparing a component A and a component B respectively;
the preparation method of the component A comprises the following steps:
mixing 51-52 parts of B-type hydroxyl-containing vinyl silicone oil, 1.5-3.5 parts of A-type hydroxyl-containing vinyl silicone oil and 0.1-0.3 part of a catalyst to obtain a first mixture;
adding 4-7.5 parts of white carbon black into the first mixture, and mixing to obtain a second mixture;
sequentially adding 12.5-17.5 parts of flame retardant and 17.5-22.5 parts of aluminum hydroxide into the second mixture, and mixing to obtain a component A;
the preparation method of the component B comprises the following steps:
mixing 48-49 parts of B-type hydroxyl-containing vinyl silicone oil, 1.5-3.5 parts of A-type hydroxyl-containing vinyl silicone oil, 8-12 parts of low-hydrogen-containing silicone oil and 0.1-0.3 part of inhibitor to obtain a third mixture;
adding 4-7.5 parts of white carbon black into the third mixture, and mixing to obtain a fourth mixture;
sequentially adding 12.5-17.5 parts of flame retardant and 17.5-22.5 parts of aluminum hydroxide into the fourth mixture, and mixing to obtain a component B;
and S2, mixing the component A and the component B to obtain the silicone rubber.
8. The method for preparing silicone rubber according to claim 7, wherein the method for preparing the A component specifically comprises:
mixing 51.9 parts of the hydroxyl-containing vinyl silicone oil of the formula B, 2.5 parts of the hydroxyl-containing vinyl silicone oil of the formula A and 0.2 part of a catalyst to obtain a first mixture;
adding 5 parts of white carbon black into the first mixture, and mixing to obtain a second mixture;
sequentially adding 15 parts of flame retardant and 20 parts of aluminum hydroxide into the second mixture, and mixing to obtain a component A;
the preparation method of the component B comprises the following specific steps:
mixing 48.1 parts of the hydroxyl-containing vinyl silicone oil of the formula B, 2.5 parts of the hydroxyl-containing vinyl silicone oil of the formula A, 10 parts of low-hydrogen-containing silicone oil and 0.2 part of an inhibitor to obtain a third mixture;
adding 5 parts of white carbon black into the third mixture, and mixing to obtain a fourth mixture;
and adding 15 parts of flame retardant and 20 parts of aluminum hydroxide into the fourth mixture in sequence, and mixing to obtain a component B.
9. The method for preparing silicone rubber according to claim 8, wherein the method for preparing the a component specifically comprises:
mixing 51.9 parts of a B-type hydroxyl-containing vinyl silicone oil with the viscosity of 30 pas, 2.5 parts of an A-type hydroxyl-containing vinyl silicone oil, 0.2 part of a catalyst and 0.2 part of a tackifier to obtain a first mixture;
adding 5 parts of white carbon black into the first mixture, and mixing to obtain a second mixture;
sequentially adding 15 parts of flame retardant and 20 parts of aluminum hydroxide into the second mixture, and mixing to obtain a component A;
the preparation method of the component B comprises the following specific steps:
mixing 48.1 parts of a hydroxyl-containing vinyl silicone oil of formula B having a viscosity of 30 pas, 2.5 parts of a hydroxyl-containing vinyl silicone oil of formula A, 10 parts of a low-hydrogen-containing silicone oil having a high viscosity, and 0.2 part of an inhibitor to obtain a third mixture;
adding 5 parts of white carbon black into the third mixture, and mixing to obtain a fourth mixture;
and adding 15 parts of flame retardant and 20 parts of aluminum hydroxide into the fourth mixture in sequence, and mixing to obtain a component B.
10. The method for preparing silicone rubber according to claim 7, wherein the method for preparing the B component specifically comprises:
mixing 48-49 parts of B-type hydroxyl-containing vinyl silicone oil, 1.5-3.5 parts of A-type hydroxyl-containing vinyl silicone oil, 8-12 parts of low-hydrogen-containing silicone oil and 0.1-0.3 part of inhibitor to obtain a third mixture;
adding 4-7.5 parts of white carbon black into the third mixture, and mixing to obtain a fourth mixture;
and sequentially adding 12.5-17.5 parts of flame retardant, 1-2 parts of color paste and 17.5-22.5 parts of aluminum hydroxide into the fourth mixture, and mixing to obtain a component B.
11. A varistor, characterized in that the encapsulant of the varistor is the silicone rubber according to any of claims 1 to 6.
12. The preparation method of the piezoresistor is characterized by comprising the following steps of:
placing a piezoresistor to be processed in a mould;
injecting the silicon rubber of any one of claims 1 to 6 into the mold, closing the silicon rubber and the piezoresistor to be processed, and demolding after molding to obtain the piezoresistor.
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| WO2022127151A1 (en) * | 2020-12-18 | 2022-06-23 | 厦门赛尔特电子有限公司 | Varistor encapsulation molding method |
| CN114685831A (en) * | 2022-02-22 | 2022-07-01 | 镇江中垒新材料科技有限公司 | Novel silica gel foaming membrane material for module sealing and shading and process |
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