CN113604051A - Vulcanized silica gel pad and manufacturing method thereof - Google Patents
Vulcanized silica gel pad and manufacturing method thereof Download PDFInfo
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Abstract
The invention relates to a silica gel sulfide pad and a manufacturing method thereof, belonging to the technical field of silica gel sulfide, comprising 100-120 parts of polyorganosiloxane, 5-10 parts of vulcanizing agent, 15-30 parts of modified nano-silica, 5-10 parts of nano-titanium dioxide, 10-20 parts of flame retardant, 1-10 parts of photoinitiator and 10-20 parts of hydrogen-containing silicone oil, wherein the modified nano-silica comprises nano-silica, isooctyl acrylate, tricarboxyphenylboronic acid, hyperbranched polyurethane acrylate, a flatting agent, an initiator and methanol; according to the invention, the modified nano silicon dioxide is added into the crude rubber, so that the compatibility with the crude rubber is excellent, the dispersibility is strong, the surface of the modified nano silicon dioxide is easy to be compatible with the crude rubber by modifying the nano silicon dioxide, the internal structure strength is high, the use of a structure regulator is reduced, compared with the traditional white carbon black, the use of an auxiliary agent is reduced, the physical property is more excellent, the modified nano silicon dioxide has a synergistic effect with the nano titanium dioxide, and the yellowing resistance and the transmittance of the vulcanized silica gel are increased.
Description
Technical Field
The invention belongs to the technical field of vulcanized silica gel, and particularly relates to a vulcanized silica gel pad and a manufacturing method thereof.
Background
The vulcanized silicone Rubber (RTV) is a new type of organosilicon elastomer which is produced in the sixties, and the most obvious characteristic of the rubber is that the rubber can be cured in situ at room temperature without heating and pressurizing, and the use is very convenient. Becomes an important component of the whole organic silicon product. The silicon sulfide rubber is a novel organic silicon elastomer, is used for manufacturing dealcoholized, deacetylated and ketoxime type single-component and two-component sealants and the like, has very good demolding performance, is particularly suitable for manufacturing precise molds, and can also be used for electronic pouring sealant as an insulating material. The existing vulcanized silica gel pad achieves the purposes of anti-yellowing and anti-aging by adding an additive with ultraviolet resistance, oxidation resistance and fatigue resistance functions or adding a light stabilizer and a mildew preventive, but the additive generally has the problems of poor compatibility and dispersibility with a silica gel matrix, so that the anti-yellowing and anti-aging functions of the silicone sealant are unstable. Therefore, the silica gel sulfide pad and the manufacturing method thereof are provided.
Disclosure of Invention
The invention aims to solve the problems and provide a vulcanized silica gel pad which is simple in structure and reasonable in design and a manufacturing method thereof.
The invention realizes the purpose through the following technical scheme:
the invention provides a silica gel sulfide pad, which comprises 100-120 parts of polyorganosiloxane, 5-10 parts of vulcanizing agent, 15-30 parts of modified nano silicon dioxide, 5-10 parts of nano titanium dioxide, 10-20 parts of flame retardant, 1-10 parts of photoinitiator and 10-20 parts of hydrogen-containing silicone oil.
As a further improvement of the invention, the modified nano-silica comprises nano-silica, isooctyl acrylate, tricarboxyphenylboronic acid, hyperbranched polyurethane acrylate, a leveling agent, an initiator and methanol.
As a further improvement of the invention, the vulcanizing agent is one or more of benzoyl peroxide, tert-butyl perbenzoate and dicumyl peroxide.
As a further improvement of the invention, one or two of antimony trioxide and aluminum hydroxide are adopted as the flame retardant.
As a further improvement of the present invention, the photoinitiator is selected from one or more of photoinitiator 819, photoinitiator 369 and photoinitiator 500.
The invention also provides a manufacturing method of the silica sulfide gel pad, which comprises the following steps:
(1) adding modified nano silicon dioxide into polysiloxane, performing ultrasonic dispersion, adding a vulcanizing agent, a flame retardant and a photoinitiator, uniformly stirring, and standing for 1-2 hours at the temperature of 40-50 ℃ to obtain a silicon rubber material;
(2) adding the silica gel material into an open mill, starting the open mill to adjust the speed ratio of a roller, adding cooling liquid at 30-40 ℃ for mixing for 20-30min, and performing cold-hot alternate circulation on the mixed product for 1-3 times to obtain a mixed material;
(3) adding nano titanium dioxide into the kneaded matter, putting the kneaded matter into an open mill again, wrapping the kneaded matter on a front roller after processing, adjusting the roller spacing along with the operation duration, and blanking and discharging after the kneaded matter is sufficiently soft and has a smooth and flat surface to obtain a silica gel pad;
(4) and pressing the silica gel pad out of the semi-finished product, and then continuously vulcanizing by hot air to obtain the vulcanized silica gel pad.
As a further improvement of the invention, the preparation process of the modified nano-silica in the step (1) is as follows:
(11) uniformly dispersing nano silicon dioxide in isooctyl acrylate in advance, adding a mixture of tricarboxyphenylboronic acid and a methanol solvent to obtain a mixed solution, preserving the temperature of the mixed solution at 40-60 ℃ for 1-2 hours, and obtaining a reaction product after centrifugal washing and freeze drying;
(12) adding the hyperbranched polyurethane acrylate, the initiator, the flatting agent and the methanol into the reaction product, and fully and uniformly mixing and stirring to obtain the modified nano silicon dioxide.
As a further improvement of the invention, the cold heat exchange circulation in the step (2) comprises the following specific steps: heating the mixed product to 65 ℃ at the speed of 2 ℃/min, preserving the heat for 20-30min, then cooling to room temperature at the speed of 5 ℃/min, and repeating the steps.
The invention has the beneficial effects that: according to the invention, the modified nano silicon dioxide is added into the crude rubber, so that the compatibility with the crude rubber is excellent, the dispersibility is strong, the surface of the modified nano silicon dioxide is easy to be compatible with the crude rubber by modifying the nano silicon dioxide, the internal structure strength is high, the use of a structure regulator is reduced, compared with the traditional white carbon black, the use of an auxiliary agent is reduced, the physical property is more excellent, the modified nano silicon dioxide has a synergistic effect with the nano titanium dioxide, and the yellowing resistance and the transmittance of the vulcanized silica gel are increased. Meanwhile, the components are connected more tightly in a cold-hot alternating mode, the formed vulcanized silica gel pad is more stable in structure, and the physical performance of the vulcanized silica gel pad is further improved.
Detailed Description
The present application is described in further detail below, and it should be noted that the following detailed description is provided for illustrative purposes only, and is not intended to limit the scope of the present application, which is defined by the appended claims.
Example 1
The silica gel vulcanizing pad of the embodiment comprises 100 parts of polysiloxane, 5 parts of vulcanizing agent, 15 parts of modified nano-silica, 5 parts of nano-titanium dioxide, 10 parts of flame retardant and 5 parts of photoinitiator, and the preparation method comprises the following steps:
(1) preparing modified nano silicon dioxide: uniformly dispersing 10 parts of nano silicon dioxide in isooctyl acrylate in advance, adding 2 parts of a mixture of 30 mass percent tricarboxyphenylboronic acid and a methanol solvent to obtain a mixed solution, preserving the temperature of the mixed solution for 1 hour at 60 ℃, and obtaining a reaction product after centrifugal washing and freeze drying; adding 5 parts of hyperbranched polyurethane acrylate, 2 parts of initiator and 2 parts of flatting agent into the reaction product, adding a proper amount of methanol, mixing and stirring uniformly to obtain modified nano silicon dioxide;
(2) preparing a silica gel material: adding modified nano silicon dioxide into polysiloxane, performing ultrasonic dispersion, adding a vulcanizing agent, a flame retardant, hydrogen-containing silicone oil and a photoinitiator, uniformly stirring, and standing for 2 hours at the temperature of 50 ℃ to obtain a silicone rubber material;
(3) preparing a vulcanized silica gel pad: adding a silica gel material into an open mill, starting the open mill to adjust the speed ratio of a roller to 1.2-1.4, then adding cooling liquid at 30 ℃ for mixing, wherein the mixing time is 30min, and after mixing, performing cold-hot alternate circulation on the product for 1 time, heating the mixed product to 65 ℃ at the speed of 2 ℃/min, preserving the heat for 20-30min, then cooling to room temperature at the speed of 5 ℃/min, and performing the circulation to obtain a mixed product; adding nano titanium dioxide into the kneaded matter, putting the kneaded matter into an open mill again, wrapping the kneaded matter on a front roller after processing, adjusting the roller spacing along with the operation duration, and blanking and discharging after the kneaded matter is sufficiently soft and has a smooth and flat surface to obtain a silica gel pad; and pressing the silica gel pad out of the semi-finished product, and then continuously vulcanizing by hot air to obtain the vulcanized silica gel pad.
Example 2
The silica gel pad of the present example includes 110 parts of polyorganosiloxane, 5 parts of vulcanizing agent, 20 parts of modified nano-silica, 8 parts of nano-titania, 10 parts of flame retardant, 5 parts of photoinitiator, and 10 parts of hydrogen-containing silicone oil, and the preparation method is as in example 1.
Example 3
The silica gel pad of the present embodiment includes 120 parts of polyorganosiloxane, 10 parts of vulcanizing agent, 30 parts of modified nano-silica, 10 parts of nano-titania, 10 parts of flame retardant, and 6 parts of photoinitiator, and the manufacturing method is as in embodiment 1.
Example 4
The silica gel sulfide pad of the embodiment comprises 110 parts of polysiloxane, 10 parts of vulcanizing agent, 30 parts of modified nano-silica, 10 parts of nano-titanium dioxide, 10 parts of flame retardant, 6 parts of photoinitiator and 10 parts of hydrogen-containing silicone oil, and the preparation method comprises the following steps:
(1) preparing modified nano silicon dioxide: uniformly dispersing 10 parts of nano silicon dioxide in isooctyl acrylate in advance, adding 2 parts of a mixture of 30 mass percent tricarboxyphenylboronic acid and a methanol solvent to obtain a mixed solution, preserving the temperature of the mixed solution for 1 hour at 60 ℃, and obtaining a reaction product after centrifugal washing and freeze drying; adding 5 parts of hyperbranched polyurethane acrylate, 2 parts of initiator and 2 parts of flatting agent into the reaction product, adding a proper amount of methanol, mixing and stirring uniformly to obtain modified nano silicon dioxide;
(2) preparing a silica gel material: adding modified nano silicon dioxide into polysiloxane, performing ultrasonic dispersion, adding a vulcanizing agent, a flame retardant, hydrogen-containing silicone oil and a photoinitiator, uniformly stirring, and standing for 2 hours at the temperature of 50 ℃ to obtain a silicone rubber material;
(3) preparing a vulcanized silica gel pad: adding a silica gel material into an open mill, starting the open mill to adjust the speed ratio of a roller to 1.2-1.4, then adding cooling liquid at 30 ℃ for mixing, wherein the mixing time is 30min, and after mixing, performing cold-hot alternate circulation on the product for 2 times, heating the mixed product to 65 ℃ at the speed of 2 ℃/min, preserving heat for 20-30min, then cooling to room temperature at the speed of 5 ℃/min, and performing the circulation to obtain a mixed product; adding nano titanium dioxide into the kneaded matter, putting the kneaded matter into an open mill again, wrapping the kneaded matter on a front roller after processing, adjusting the roller spacing along with the operation duration, and blanking and discharging after the kneaded matter is sufficiently soft and has a smooth and flat surface to obtain a silica gel pad; and pressing the silica gel pad out of the semi-finished product, and then continuously vulcanizing by hot air to obtain the vulcanized silica gel pad.
Example 5
The silica gel sulfide pad of the embodiment comprises 110 parts of polysiloxane, 10 parts of vulcanizing agent, 30 parts of modified nano-silica, 10 parts of nano-titanium dioxide, 10 parts of flame retardant, 6 parts of photoinitiator and 10 parts of hydrogen-containing silicone oil, and the preparation method comprises the following steps:
(1) preparing modified nano silicon dioxide: uniformly dispersing 10 parts of nano silicon dioxide in isooctyl acrylate in advance, adding 2 parts of a mixture of 30 mass percent tricarboxyphenylboronic acid and a methanol solvent to obtain a mixed solution, preserving the temperature of the mixed solution for 1 hour at 60 ℃, and obtaining a reaction product after centrifugal washing and freeze drying; adding 5 parts of hyperbranched polyurethane acrylate, 2 parts of initiator and 2 parts of flatting agent into the reaction product, adding a proper amount of methanol, mixing and stirring uniformly to obtain modified nano silicon dioxide;
(2) preparing a silica gel material: adding modified nano silicon dioxide into polysiloxane, performing ultrasonic dispersion, adding a vulcanizing agent, a flame retardant, hydrogen-containing silicone oil and a photoinitiator, uniformly stirring, and standing for 2 hours at the temperature of 50 ℃ to obtain a silicone rubber material;
(3) preparing a vulcanized silica gel pad: adding a silica gel material into an open mill, starting the open mill to adjust the speed ratio of a roller to 1.2-1.4, then adding cooling liquid at 30 ℃ for mixing, wherein the mixing time is 30min, and after mixing, performing cold-hot alternate circulation on the product for 3 times, heating the mixed product to 65 ℃ at the speed of 2 ℃/min, preserving the heat for 20-30min, then cooling to room temperature at the speed of 5 ℃/min, and performing the circulation to obtain a mixed product; adding nano titanium dioxide into the kneaded matter, putting the kneaded matter into an open mill again, wrapping the kneaded matter on a front roller after processing, adjusting the roller spacing along with the operation duration, and blanking and discharging after the kneaded matter is sufficiently soft and has a smooth and flat surface to obtain a silica gel pad; and pressing the silica gel pad out of the semi-finished product, and then continuously vulcanizing by hot air to obtain the vulcanized silica gel pad.
Example 6
The silica gel vulcanizing pad of the embodiment comprises 110 parts of polysiloxane, 10 parts of vulcanizing agent, 30 parts of modified nano silicon dioxide, 15 parts of nano titanium dioxide, 10 parts of flame retardant, 6 parts of photoinitiator and 5 parts of coloring agent, and the preparation method comprises the following steps:
(1) preparing modified nano silicon dioxide: uniformly dispersing 10 parts of nano silicon dioxide in isooctyl acrylate in advance, adding 2 parts of a mixture of 30 mass percent tricarboxyphenylboronic acid and a methanol solvent to obtain a mixed solution, preserving the temperature of the mixed solution for 1 hour at 60 ℃, and obtaining a reaction product after centrifugal washing and freeze drying; adding 5 parts of hyperbranched polyurethane acrylate, 2 parts of initiator and 2 parts of flatting agent into the reaction product, adding a proper amount of methanol, mixing and stirring uniformly to obtain modified nano silicon dioxide;
(2) preparing a silica gel material: adding modified nano silicon dioxide into polysiloxane, performing ultrasonic dispersion, adding a vulcanizing agent, a flame retardant, a photoinitiator, hydrogen-containing silicone oil and a colorant, uniformly stirring, and standing for 2 hours at the temperature of 50 ℃ to obtain a silicone rubber material;
(3) preparing a vulcanized silica gel pad: adding a silica gel material into an open mill, starting the open mill to adjust the speed ratio of a roller to 1.2-1.4, then adding cooling liquid at 30 ℃ for mixing, wherein the mixing time is 30min, and after mixing, performing cold-hot alternate circulation on the product for 2 times, heating the mixed product to 65 ℃ at the speed of 2 ℃/min, preserving heat for 20-30min, then cooling to room temperature at the speed of 5 ℃/min, and performing the circulation to obtain a mixed product; adding nano titanium dioxide into the kneaded matter, putting the kneaded matter into an open mill again, wrapping the kneaded matter on a front roller after processing, adjusting the roller spacing along with the operation duration, and blanking and discharging after the kneaded matter is sufficiently soft and has a smooth and flat surface to obtain a silica gel pad; and pressing the silica gel pad out of the semi-finished product, and then continuously vulcanizing by hot air to obtain the vulcanized silica gel pad.
Comparative example 1
The silica gel sulfide pad of the embodiment comprises 110 parts of polysiloxane, 10 parts of vulcanizing agent, 10 parts of flame retardant, 6 parts of photoinitiator and 10 parts of hydrogen-containing silicone oil, and the preparation method comprises the following steps:
(1) preparing a silica gel material: carrying out ultrasonic dispersion on polysiloxane, adding a vulcanizing agent, a flame retardant, hydrogen-containing silicone oil and a photoinitiator, uniformly stirring, and standing for 2 hours at the temperature of 50 ℃ to obtain a silicone rubber material;
(2) preparing a vulcanized silica gel pad: adding a silica gel material into an open mill, starting the open mill to adjust the speed ratio of a roller to 1.2-1.4, then adding cooling liquid at 30 ℃ for mixing, wherein the mixing time is 30min, and after mixing, performing cold-hot alternate circulation on the product for 2 times, heating the mixed product to 65 ℃ at the speed of 2 ℃/min, preserving heat for 20-30min, then cooling to room temperature at the speed of 5 ℃/min, and performing the circulation to obtain a mixed product; putting the kneaded material into an open mill again, wrapping the kneaded material on a front roller after processing, adjusting the roller spacing along with the operation duration, and blanking and discharging pieces after the kneaded material is sufficiently soft and has a smooth and flat surface to obtain a silica gel pad; and pressing the silica gel pad out of the semi-finished product, and then continuously vulcanizing by hot air to obtain the vulcanized silica gel pad.
Comparative example 2
The silica gel sulfide pad of the embodiment comprises 110 parts of polysiloxane, 10 parts of vulcanizing agent, 10 parts of nano titanium dioxide, 10 parts of flame retardant, 6 parts of photoinitiator and 10 parts of hydrogen-containing silicone oil, and the preparation method comprises the following steps:
(1) preparing a silica gel material: carrying out ultrasonic dispersion on polysiloxane, adding a vulcanizing agent, a flame retardant and a photoinitiator, uniformly stirring, and standing for 2 hours at the temperature of 50 ℃ to obtain a silicon rubber material;
(2) preparing a vulcanized silica gel pad: adding a silica gel material into an open mill, starting the open mill to adjust the speed ratio of a roller to 1.2-1.4, then adding cooling liquid at 30 ℃ for mixing, wherein the mixing time is 30min, and after mixing, performing cold-hot alternate circulation on the product for 2 times, heating the mixed product to 65 ℃ at the speed of 2 ℃/min, preserving heat for 20-30min, then cooling to room temperature at the speed of 5 ℃/min, and performing the circulation to obtain a mixed product; adding nano titanium dioxide into the kneaded matter, putting the kneaded matter into an open mill again, wrapping the kneaded matter on a front roller after processing, adjusting the roller spacing along with the operation duration, and blanking and discharging after the kneaded matter is sufficiently soft and has a smooth and flat surface to obtain a silica gel pad; and pressing the silica gel pad out of the semi-finished product, and then continuously vulcanizing by hot air to obtain the vulcanized silica gel pad.
Comparative example 3
The silica gel sulfide pad of the embodiment comprises 110 parts of polysiloxane, 10 parts of vulcanizing agent, 30 parts of white carbon black, 5 parts of structure regulator, 10 parts of nano titanium dioxide, 10 parts of flame retardant, 6 parts of photoinitiator, 10 parts of hydrogen-containing silicone oil and 5 parts of coloring agent, and the manufacturing method comprises the following steps:
(1) preparing a silica gel material: adding white carbon black into polyorganosiloxane, performing ultrasonic dispersion, adding a vulcanizing agent, a flame retardant, hydrogen-containing silicone oil and a photoinitiator, uniformly stirring, and standing for 2 hours at the temperature of 50 ℃ to obtain a silicone material;
(2) preparing a vulcanized silica gel pad: adding a silica gel material into an open mill, starting the open mill to adjust the speed ratio of a roller to 1.2-1.4, then adding cooling liquid at 30 ℃ for mixing, wherein the mixing time is 30min, and after mixing, performing cold-hot alternate circulation on the product for 2 times, heating the mixed product to 65 ℃ at the speed of 2 ℃/min, preserving heat for 20-30min, then cooling to room temperature at the speed of 5 ℃/min, and performing the circulation to obtain a mixed product; adding nano titanium dioxide into the kneaded matter, putting the kneaded matter into an open mill again, wrapping the kneaded matter on a front roller after processing, adjusting the roller spacing along with the operation duration, and blanking and discharging after the kneaded matter is sufficiently soft and has a smooth and flat surface to obtain a silica gel pad; and pressing the silica gel pad out of the semi-finished product, and then continuously vulcanizing by hot air to obtain the vulcanized silica gel pad.
Comparative example 4
The silica gel sulfide pad of the embodiment comprises 110 parts of polysiloxane, 10 parts of vulcanizing agent, 30 parts of modified nano-silica, 10 parts of flame retardant, 6 parts of photoinitiator, 10 parts of hydrogen-containing silicone oil and 5 parts of coloring agent, and the preparation method comprises the following steps:
(1) preparing modified nano silicon dioxide: uniformly dispersing 10 parts of nano silicon dioxide in isooctyl acrylate in advance, adding 2 parts of a mixture of 30 mass percent tricarboxyphenylboronic acid and a methanol solvent to obtain a mixed solution, preserving the temperature of the mixed solution for 1 hour at 60 ℃, and obtaining a reaction product after centrifugal washing and freeze drying; adding 5 parts of hyperbranched polyurethane acrylate, 2 parts of initiator and 2 parts of flatting agent into the reaction product, adding a proper amount of methanol, mixing and stirring uniformly to obtain modified nano silicon dioxide;
(2) preparing a silica gel material: adding modified nano silicon dioxide into polysiloxane, performing ultrasonic dispersion, adding a vulcanizing agent, a flame retardant, hydrogen-containing silicone oil and a photoinitiator, uniformly stirring, and standing for 2 hours at the temperature of 50 ℃ to obtain a silicone rubber material;
(3) preparing a vulcanized silica gel pad: adding a silica gel material into an open mill, starting the open mill to adjust the speed ratio of a roller to 1.2-1.4, then adding cooling liquid at 30 ℃ for mixing, wherein the mixing time is 30min, and after mixing, performing cold-hot alternate circulation on the product for 2 times, heating the mixed product to 65 ℃ at the speed of 2 ℃/min, preserving heat for 20-30min, then cooling to room temperature at the speed of 5 ℃/min, and performing the circulation to obtain a mixed product; putting the kneaded material into an open mill again, wrapping the kneaded material on a front roller after processing, adjusting the roller spacing along with the operation duration, and blanking and discharging pieces after the kneaded material is sufficiently soft and has a smooth and flat surface to obtain a silica gel pad; and pressing the silica gel pad out of the semi-finished product, and then continuously vulcanizing by hot air to obtain the vulcanized silica gel pad.
Comparative example 5
The silica gel sulfide pad of the embodiment comprises 110 parts of polysiloxane, 10 parts of vulcanizing agent, 30 parts of modified nano-silica, 10 parts of nano-titanium dioxide, 10 parts of flame retardant, 6 parts of photoinitiator and 10 parts of hydrogen-containing silicone oil, and the preparation method comprises the following steps:
(1) preparing modified nano silicon dioxide: uniformly dispersing 10 parts of nano silicon dioxide in isooctyl acrylate in advance, adding 2 parts of a mixture of 30 mass percent tricarboxyphenylboronic acid and a methanol solvent to obtain a mixed solution, preserving the temperature of the mixed solution for 1 hour at 60 ℃, and obtaining a reaction product after centrifugal washing and freeze drying; adding 5 parts of hyperbranched polyurethane acrylate, 2 parts of initiator and 2 parts of flatting agent into the reaction product, adding a proper amount of methanol, mixing and stirring uniformly to obtain modified nano silicon dioxide;
(2) preparing a silica gel material: adding modified nano silicon dioxide into polysiloxane, performing ultrasonic dispersion, adding a vulcanizing agent, a flame retardant, hydrogen-containing silicone oil and a photoinitiator, uniformly stirring, and standing for 2 hours at the temperature of 50 ℃ to obtain a silicone rubber material;
(3) preparing a vulcanized silica gel pad: adding a silica gel material into an open mill, starting the open mill to adjust the speed ratio of a roller to 1.2-1.4, then adding cooling liquid at 30 ℃ for mixing for 30min, cooling the product after mixing to room temperature to obtain a mixed product; adding nano titanium dioxide into the kneaded matter, putting the kneaded matter into an open mill again, wrapping the kneaded matter on a front roller after processing, adjusting the roller spacing along with the operation duration, and blanking and discharging after the kneaded matter is sufficiently soft and has a smooth and flat surface to obtain a silica gel pad; and pressing the silica gel pad out of the semi-finished product, and then continuously vulcanizing by hot air to obtain the vulcanized silica gel pad.
Comparative example 6
The silica gel sulfide pad of the embodiment comprises 110 parts of polysiloxane, 10 parts of vulcanizing agent, 30 parts of modified nano-silica, 10 parts of nano-titanium dioxide, 10 parts of flame retardant, 6 parts of photoinitiator and 10 parts of hydrogen-containing silicone oil, and the preparation method comprises the following steps:
(1) preparing modified nano silicon dioxide: uniformly dispersing 10 parts of nano silicon dioxide in isooctyl acrylate in advance, adding 2 parts of a mixture of 30 mass percent tricarboxyphenylboronic acid and a methanol solvent to obtain a mixed solution, preserving the temperature of the mixed solution for 1 hour at 60 ℃, and obtaining a reaction product after centrifugal washing and freeze drying; adding 5 parts of hyperbranched polyurethane acrylate, 2 parts of initiator and 2 parts of flatting agent into the reaction product, adding a proper amount of methanol, mixing and stirring uniformly to obtain modified nano silicon dioxide;
(2) preparing a silica gel material: adding modified nano silicon dioxide into polysiloxane, performing ultrasonic dispersion, adding a vulcanizing agent, a flame retardant and a photoinitiator, uniformly stirring, and standing for 2 hours at the temperature of 50 ℃ to obtain a silicon rubber material;
(3) preparing a vulcanized silica gel pad: adding a silica gel material into an open mill, starting the open mill to adjust the speed ratio of a roller to 1.2-1.4, then adding cooling liquid at 30 ℃ for mixing, wherein the mixing time is 30min, and after mixing, performing cold-hot alternate circulation on the product for 4 times, heating the mixed product to 65 ℃ at the speed of 2 ℃/min, preserving heat for 20-30min, then cooling to room temperature at the speed of 5 ℃/min, and performing the circulation to obtain a mixed product; adding nano titanium dioxide into the kneaded matter, putting the kneaded matter into an open mill again, wrapping the kneaded matter on a front roller after processing, adjusting the roller spacing along with the operation duration, and blanking and discharging after the kneaded matter is sufficiently soft and has a smooth and flat surface to obtain a silica gel pad; and pressing the silica gel pad out of the semi-finished product, and then continuously vulcanizing by hot air to obtain the vulcanized silica gel pad.
Comparative example 7
The silica gel sulfide pad of the embodiment comprises 110 parts of polysiloxane, 10 parts of vulcanizing agent, 30 parts of modified nano-silica, 10 parts of nano-titanium dioxide, 10 parts of flame retardant, 6 parts of photoinitiator and 10 parts of hydrogen-containing silicone oil, and the preparation method comprises the following steps:
(1) preparing modified nano silicon dioxide: uniformly dispersing 10 parts of nano silicon dioxide in isooctyl acrylate in advance, preserving heat for 1h at the temperature of 60 ℃, and obtaining a reaction product after centrifugal washing and freeze drying; adding 5 parts of hyperbranched polyurethane acrylate, 2 parts of initiator and 2 parts of flatting agent into the reaction product, adding a proper amount of methanol, mixing and stirring uniformly to obtain modified nano silicon dioxide;
(2) preparing a silica gel material: adding modified nano silicon dioxide into polysiloxane, performing ultrasonic dispersion, adding a vulcanizing agent, a flame retardant, hydrogen-containing silicone oil and a photoinitiator, uniformly stirring, and standing for 2 hours at the temperature of 50 ℃ to obtain a silicone rubber material;
(3) preparing a vulcanized silica gel pad: adding a silica gel material into an open mill, starting the open mill to adjust the speed ratio of a roller to 1.2-1.4, then adding cooling liquid at 30 ℃ for mixing, wherein the mixing time is 30min, and after mixing, performing cold-hot alternate circulation on the product for 2 times, heating the mixed product to 65 ℃ at the speed of 2 ℃/min, preserving heat for 20-30min, then cooling to room temperature at the speed of 5 ℃/min, and performing the circulation to obtain a mixed product; adding nano titanium dioxide into the kneaded matter, putting the kneaded matter into an open mill again, wrapping the kneaded matter on a front roller after processing, adjusting the roller spacing along with the operation duration, and blanking and discharging after the kneaded matter is sufficiently soft and has a smooth and flat surface to obtain a silica gel pad; and pressing the silica gel pad out of the semi-finished product, and then continuously vulcanizing by hot air to obtain the vulcanized silica gel pad.
Comparative example 8
The silica gel sulfide pad of this example includes 110 parts of polyorganosiloxane, 10 parts of vulcanizing agent, 10 parts of modified nano-silica, 5 parts of nano-titania, 10 parts of flame retardant, 6 parts of photoinitiator, 5 parts of colorant, and 10 parts of hydrogen-containing silicone oil, and the manufacturing method is the same as example 6.
First, the following table shows the performance parameters of the silica gel pads prepared in examples 1 to 6 and comparative examples 1 to 7, which were measured by a conventional method:
TABLE 1 physical Properties of the silica gel pad
Secondly, detecting the yellowing index and the transmittance of the silica sulfide gel pads prepared in the examples 1-5 and the comparative examples 1-7 by adopting a whiteness meter and a 722 spectrophotometer respectively, wherein the yellowing index and the transmittance are measured after photo-oxidative aging for 48 hours, and the measurement data are shown in the following table:
TABLE 2 yellowing index and transmittance of silica sulfide gel pads
As can be seen from the data in table 1, the addition of the modified nano-silica in the invention can replace the effect of white carbon black, so that the silica sulfide mat can achieve the same or more excellent physical properties, no structural additive needs to be added, and the physical properties of the silica sulfide mat can be further improved by adopting a specific preparation method; as can be seen from the data in table 2, although the modified nano-silica and the common white carbon black have little change in physical properties, the modified nano-silica used in the present invention enables the silica gel vulcanized pad to have an excellent anti-yellowing effect, and meanwhile, as can be seen from example 4, comparative example 2 and comparative example 4, the modified nano-silica and the nano-titania used in the present application can both significantly improve the anti-yellowing property and the transmittance of the silica gel vulcanized pad, and both synergistically have a more excellent effect.
And thirdly, testing the silica gel pads prepared in the example 6 and the comparative examples 3, 4 and 8 by using a colorimeter, wherein the initial chromaticities of the two groups of silica gel pads are measured and recorded as S1, and then the chromaticities of the two groups of silica gel pads are tested and recorded as S2 after the two groups of silica gel pads are subjected to ultraviolet aging in a box for 48 hours, wherein the decoloration rate is (S1-S2)/S1 multiplied by 100%.
TABLE 3 decolorization test
| Item | Example 6 | Comparative example 3 | Comparative example 4 | Comparative example 8 |
| Decolorization ratio | 1.1％ | 3.5％ | 3.9％ | 1.7％ |
As can be seen from the above table, the decoloring rates of the comparative examples 3 and 4 are greater than those of the example 6, which shows that both the modified nano-silica and the nano-titania in the silica gel sulfide pad have a beneficial effect on the decoloring rate of the silica gel sulfide, and the silica gel sulfide pad of the present invention has excellent color-locking performance.
The above-mentioned embodiments only express several embodiments of the present invention, and the description thereof is more specific and detailed, but not construed as limiting the scope of the present invention. It should be noted that, for a person skilled in the art, several variations and modifications can be made without departing from the inventive concept, which falls within the scope of the present invention.
Claims (8)
1. The silica gel sulfide pad is characterized by comprising, by weight, 100-120 parts of polyorganosiloxane, 5-10 parts of a vulcanizing agent, 15-30 parts of modified nano-silica, 5-10 parts of nano-titanium dioxide, 10-20 parts of a flame retardant, 1-10 parts of a photoinitiator and 10-20 parts of hydrogen-containing silicone oil.
2. The silica gel pad according to claim 1, wherein the modified nano-silica comprises nano-silica, isooctyl acrylate, tricarboxyphenylboronic acid, hyperbranched urethane acrylate, a leveling agent, an initiator, and methanol.
3. The silica gel pad of claim 1, wherein the vulcanizing agent is one or more of benzoyl peroxide, t-butyl perbenzoate, and dicumyl peroxide.
4. The silica gel pad according to claim 1, wherein the flame retardant is one or two of antimony trioxide and aluminum hydroxide.
5. The silica gel pad according to claim 3, wherein the photoinitiator is selected from one or more of photoinitiator 819, photoinitiator 369 and photoinitiator 500.
6. The method for manufacturing the silica gel vulcanization pad according to any one of claims 1 to 5, characterized by comprising the steps of:
(1) adding modified nano silicon dioxide into polysiloxane, performing ultrasonic dispersion, adding a vulcanizing agent, a flame retardant and a photoinitiator, uniformly stirring, and standing for 1-2 hours at the temperature of 40-50 ℃ to obtain a silicon rubber material;
(2) adding the silica gel material into an open mill, starting the open mill to adjust the speed ratio of a roller, adding cooling liquid at 30-40 ℃ for mixing for 20-30min, and performing cold-hot alternate circulation on the mixed product for 1-3 times to obtain a mixed material;
(3) adding nano titanium dioxide into the kneaded matter, putting the kneaded matter into an open mill again, wrapping the kneaded matter on a front roller after processing, adjusting the roller spacing along with the operation duration, and blanking and discharging after the kneaded matter is sufficiently soft and has a smooth and flat surface to obtain a silica gel pad;
(4) and pressing the silica gel pad out of the semi-finished product, and then continuously vulcanizing by hot air to obtain the vulcanized silica gel pad.
7. The method for manufacturing the silica gel pad according to claim 6, wherein the modified nano-silica in the step (1) is prepared by the following steps:
(11) uniformly dispersing nano silicon dioxide in isooctyl acrylate in advance, adding a mixture of tricarboxyphenylboronic acid and a methanol solvent to obtain a mixed solution, preserving the temperature of the mixed solution at 40-60 ℃ for 1-2 hours, and obtaining a reaction product after centrifugal washing and freeze drying;
(12) adding the hyperbranched polyurethane acrylate, the initiator, the flatting agent and the methanol into the reaction product, and fully and uniformly mixing and stirring to obtain the modified nano silicon dioxide.
8. The method for manufacturing the silica gel mat according to claim 6, wherein the cold-heat exchange circulation in the step (2) comprises the following specific steps: heating the mixed product to 65 ℃ at the speed of 2 ℃/min, preserving the heat for 20-30min, then cooling to room temperature at the speed of 5 ℃/min, and repeating the steps.
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