CN111607237A - Preparation method of silica gel-like product material - Google Patents

Preparation method of silica gel-like product material Download PDF

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CN111607237A
CN111607237A CN202010541137.3A CN202010541137A CN111607237A CN 111607237 A CN111607237 A CN 111607237A CN 202010541137 A CN202010541137 A CN 202010541137A CN 111607237 A CN111607237 A CN 111607237A
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silica gel
nickel boride
bisphenol
silyl
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陈翔翔
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Pujiang Yuyang Plastic Co ltd
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    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08LCOMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L91/00Compositions of oils, fats or waxes; Compositions of derivatives thereof
    • C08L91/06Waxes
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    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00Use of inorganic substances as compounding ingredients
    • C08K3/18Oxygen-containing compounds, e.g. metal carbonyls
    • C08K3/24Acids; Salts thereof
    • C08K3/26Carbonates; Bicarbonates
    • C08K2003/265Calcium, strontium or barium carbonate
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K2201/00Specific properties of additives
    • C08K2201/002Physical properties
    • C08K2201/003Additives being defined by their diameter
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K2201/00Specific properties of additives
    • C08K2201/011Nanostructured additives
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08LCOMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2205/00Polymer mixtures characterised by other features
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Abstract

The invention relates to the field of material processing, in particular to a preparation method of a silica gel-like product material; the components of the composition comprise: SEBS, paraffin oil, polypropylene, silicone master batch, an antioxidant, calcium powder and bisphenol silyl nano nickel boride; the invention provides bisphenol silyl nano nickel boride, which is used in combination with silicone master batches to effectively improve the dispersibility of calcium powder filler, so that the calcium powder filler has good stability and non-migration property; the melting rate and the deformability of the material are effectively improved, the viscosity is reduced, the plasticization is improved, the melt is prevented from bursting, the smooth feeling, the glossiness and the touch feeling of the surface of the material are improved, and the material is closer to a silica gel product in appearance; the material of the invention is similar to a silica gel product in appearance, touch and mechanical properties, is a substitute product of the silica gel product with low cost and simple process, and has economic value.

Description

Preparation method of silica gel-like product material
Technical Field
The invention relates to the field of material processing, in particular to a preparation method of a silica gel-like product material.
Background
The silicon rubber can be classified into a condensation type, an addition type (platinum catalysis) and a free radical curing type (peroxide catalysis) according to different vulcanization crosslinking modes. The addition type silicone rubber has the advantages of no low molecular by-product coming out in the vulcanization process, stable size (small linear shrinkage rate) of a cured product, uniform curing film forming, no influence on electrical performance, easy control of curing conditions, high conversion rate and the like, and is widely applied in various industries, particularly in the electronic field.
CN105224034A discloses a preparation method of a double-layer silica gel coated PC panel, which comprises the following steps: (1) drilling four positioning holes on the periphery of the prepared elastic PC flat plate; (2) coating glue on two sides of the elastic PC flat plate, and then putting the elastic PC flat plate into an oven for drying; (3) coating two pieces of silica gel with the same thickness on two sides of the elastic PC flat plate respectively, putting the elastic PC flat plate coated with the silica gel material into a mold core, and matching a positioning hole of the elastic PC flat plate with a positioning needle of the mold core; (4) and (3) carrying out die assembly molding, wherein the silica gel forms the elastic silica gel covering layer, the two elastic silica gel covering layers are formed, the thicknesses of the two elastic silica gel covering layers are consistent, and the elastic PC panel is positioned in the middle of the two elastic silica gel covering layers. The invention also discloses a PC panel. The invention ensures the hand feeling of the silica gel through the elastic PC flat plate and has the strength flatness of the PC plate; 4 positioning holes are formed in the elastic PC panel to ensure that the elastic PC panel is wrapped in the middle of a product, and the product is not dislocated and is formed by one-step compression molding, so that a double-layer silica gel-wrapped PC panel without a bonding line is formed.
CN102115605B discloses an in-situ reinforced and heat-conducting modified LED packaging silica gel and a preparation method thereof: adding a certain amount of mixed solution of tetraalkoxysilane and a plurality of metal tetraalkoxy compounds into high refractive index methyl phenyl vinyl silicone oil containing a proper amount of solvent and catalyst, reacting with deionized water for a period of time under a certain condition, and removing the catalyst, the solvent and unreacted water to obtain vinyl glue; the vinyl rubber is mixed with methyl phenyl hydrogen-containing silicone oil, a platinum catalyst and an inhibitor according to a certain proportion to prepare the LED packaging silicone rubber. The refractive index of the LED packaging silicon rubber is more than 1.50, the tensile strength is 0-4.8 Mpa, the thermal conductivity is 0.2-1.8W/m "K, the light transmittance is more than 95%, the light attenuation is less than 6% after the ultraviolet radiation is carried out for 1002 hours, and the LED packaging silicon rubber is very suitable for LED packaging, especially high-power LED packaging.
CN102838871A relates to a silica gel composition, a preparation method thereof and an insulation product prepared by using the same. The silica gel composition comprises 50 percent of component A and 50 percent of component B in percentage by weight, wherein the component A comprises the following components: 65% -68% of methyl vinyl silicone rubber; 25% -28% of white carbon black; 0.1% of double five; 5% -9% of hydroxyl silicone oil; the component B is aluminum hydroxide or aluminum oxide or magnesium hydroxide or magnesium oxide or quartz sand or the mixture of any two or more of the above substances. The preparation method of the silica gel composition comprises the steps of firstly putting the components of the component A into an internal mixer in proportion for mixing, and adding the component B after a period of time for mixing until the product is uniform. The invention has the advantages that: the insulating material has good insulating effect, can be widely applied to products with high requirements on insulating effect, and has the voltage withstanding capability of 4000V.
The silica gel has excellent performance and wide application range, but the application of the silica gel is greatly limited because the production cost of the silica gel is higher compared with other resin products.
Disclosure of Invention
In order to solve the problems, the invention provides a preparation method of a silica gel-like product material.
A preparation method of a silica gel-like product material comprises the following components: 20-30 parts of polystyrene-ethylene-butadiene-styrene (SEBS), 48-56 parts of paraffin oil, 14-21 parts of polypropylene, 0.8-3.6 parts of silicone master batch, 0.5-1.8 parts of antioxidant, 8-15 parts of calcium powder and 0.08-0.36 part of bisphenol silyl nano nickel boride; the preparation scheme is as follows:
adding polystyrene-ethylene-butadiene-styrene (SEBS), bisphenol silyl nano nickel boride and silicone master batch into a high-speed mixer, slowly adding paraffin oil into the mixer under stirring, controlling the addition to be finished within 45-90min, continuing to stir for 10-60min after the addition is finished, standing for 120-180min after uniform mixing, then adding polypropylene, antioxidant and calcium powder into the mixer, and mixing at high speed for 8-16min to obtain a mixture; adding the obtained mixture into a double-screw extruder, controlling the rotating speed of a screw to be 120-; drying the obtained granules at 60-80 ℃ for 5-10h, and then carrying out injection molding to obtain the silica gel imitation product material.
The bisphenol silyl nanometer nickel boride is prepared by performing hydrosilylation reaction on modified nanometer nickel boride, tetra [ dimethylsiloxy ] silane and diallyl bisphenol.
The preparation method of the modified nano nickel boride comprises the following steps:
adding 100-300 parts by mass of 0.1-1mol/L nickel nitrate aqueous solution into a reaction kettle, bubbling with high-purity nitrogen for 5-10min to remove oxygen, controlling the temperature to 0-10 ℃, and protecting with nitrogen; and adding 3.1-4.6 parts of sodium borohydride and 4.5-7.2 parts of sodium hydroxide into 150-200 parts of pure water, mixing and stirring uniformly, slowly adding the prepared solution into a reaction kettle, controlling the addition of the solution for 180min, stirring for 1-5h at normal temperature after completion, then carrying out centrifugal filtration, washing and drying to obtain nickel boride nanoparticles, dispersing the obtained nickel boride nanoparticles into 50-120 parts of deionized water, then adding 0.1-0.5 part of coupling agent, heating to 70-100 ℃, carrying out stirring reaction for 120-180min, continuing stirring and reacting for 20-60min, cooling to normal temperature, filtering, washing, and drying to obtain the modified nano nickel boride.
The preparation method of the bisphenol silyl nano nickel boride comprises the following steps:
adding 20-35 parts of modified nano nickel boride, 1-6 parts of tetra [ dimethylsiloxane-based ] silane, 2-6 parts of diallyl bisphenol and 300 parts of solvent oil 200-90 parts by mass into a reaction kettle, heating to 75-90 ℃ under the protection of nitrogen, adding 3-7 parts of n-butyl alcohol dispersion containing 0.2-0.8 part of chloroplatinic acid into the reaction kettle, controlling the temperature to react for 70-100min, filtering after the reaction is finished, and drying to obtain the bisphenol silane-based nano nickel boride.
The partial reaction is shown as the following formula:
Figure BDA0002538891910000041
the antioxidant is bis-cinnamoyl thiodipropionate or bis-stearoyl thiodipropionate or dibutyl hydroxy toluene.
The average molecular weight of the polypropylene is 10-15 ten thousand.
The average grain diameter of the bisphenol silyl nanometer nickel boride is 0.01-0.1 mu m.
The mesh number of the calcium powder is 300-500 meshes.
The coupling agent is selected from one or more of vinyl trimethoxy silane and methacryloxypropyl trimethoxy silane.
The invention relates to a preparation method of a silica gel-like product material, which is characterized in that polystyrene-ethylene-butadiene-styrene and paraffin oil are filled with oil in a mixer under the combined action of bisphenol silyl nano nickel boride and silicone master batches provided by the invention, and then are mixed with polypropylene, a filler and other additives uniformly under a molten state, and the bisphenol silyl nano nickel boride, the additive and the silicone master batches are matched for use, so that the dispersibility of calcium powder filler can be effectively improved, and the calcium powder filler has good stability and non-migration property; the melting rate and the deformability of the material are effectively improved, the viscosity is reduced, the plasticization is improved, the melt is prevented from bursting, the smooth feeling, the glossiness and the touch feeling of the surface of the material are improved, and the material is closer to a silica gel product in appearance; the material of the invention is similar to a silica gel product in appearance, touch and mechanical properties, is a substitute product of the silica gel product with low cost and simple process, and has economic value.
Drawings
FIG. 1 is a Fourier infrared spectrum of the material of the simulated silica gel article prepared in example 2.
A stretching vibration absorption peak of a benzene ring exists near 1612/1500/1447/1377cm < -1 >, and a stretching absorption peak of hydrocarbon exists near 2962cm < -1 >, so that the styrene-ethylene-butadiene-styrene and paraffin oil participate in the reaction; a stretching vibration absorption peak of phenolic hydroxyl exists near 3344cm < -1 >, which shows that the bisphenol silyl nano nickel boride participates in the reaction; the antisymmetric stretching absorption peak of silicon oxygen exists near 1026cm < -1 >, and the stretching absorption peak of silicon carbon exists near 760cm < -1 >, so that the silicone master batch participates in the reaction; an out-of-plane bending/in-plane bending absorption peak of carbonic acid heel ions exists near 883/692cm < -1 >, which indicates that calcium powder participates in the reaction.
Detailed Description
The invention is further illustrated by the following specific examples:
the twin screw extruder used a laboratory grade HAAKE Eurolab16 bench-top parallel co-rotating twin screw extruder,
the injection molding equipment uses a JY-ZS-28 small laboratory injection molding machine.
And (3) performing tensile property test on the standard sample strip of the material by using a TCS-2000 high-speed rail tensile testing machine according to GB/T1040-2006. The tensile strength and elongation at break of the test specimen were measured by a tensile test at a tensile rate of 100 mm/min.
The product appearance adopts visual inspection and touch method.
Example 1
A preparation method of a silica gel-like product material comprises the following components: 20g of SEBS 6151, 48g of paraffin oil, 14g of polypropylene, 0.8g of silicone master batch, 0.5g of antioxidant, 8g of calcium powder and 0.08g of bisphenol silyl nano nickel boride; the preparation scheme is as follows:
adding SEBS 6151, bisphenol silyl nano nickel boride and silicone master batch into a high-speed mixer, slowly adding paraffin oil into the mixer under stirring, controlling the adding time to be 45min, continuously stirring for 10min after the adding is finished, standing for 120min after the mixing is uniform, then adding polypropylene, antioxidant and calcium powder into the mixer, and mixing at high speed for 8min to obtain a mixture; adding the obtained mixture into a double-screw extruder, controlling the rotating speed of a screw to be 120r/min, controlling the feeding speed to be 160r/min and controlling the temperature to be 185 ℃; and drying the obtained particles at 60 ℃ for 5 hours, and then carrying out injection molding to obtain the silica gel imitation product material.
Adding 100g of 0.1mol/L nickel nitrate aqueous solution into a reaction kettle, bubbling with high-purity nitrogen for 5min to remove oxygen, controlling the temperature to be 0 ℃, and protecting with nitrogen; in addition, 3.1g of sodium borohydride and 4.5g of sodium hydroxide are added into 150g of pure water, the mixed solution is slowly added into a reaction kettle after being uniformly mixed and stirred, the addition is controlled to be finished within 120min, the solution is stirred for 1h at normal temperature after the addition is finished, then centrifugal filtration is carried out, nickel boride nanoparticles are obtained after washing and drying, the obtained nickel boride nanoparticles are dispersed into 50g of deionized water, then 0.1g of vinyl trimethoxy silane is added, the temperature is increased to 70 ℃, stirring reaction is carried out for 120min, stirring reaction is continued for 180min, the reaction is carried out for 20min, the mixture is cooled to the normal temperature, and then filtration, washing and drying are carried out, thus obtaining the modified nano nickel boride.
The preparation method of the bisphenol silyl nano nickel boride comprises the following steps:
adding 20g of modified nano nickel boride, 1g of tetra [ dimethylsilyloxy alkyl ] silane, 2g of diallyl bisphenol and 200g of solvent oil into a reaction kettle, heating to 70 ℃ under the protection of nitrogen, then adding 3g of n-butyl alcohol dispersion liquid containing 0.2g of chloroplatinic acid into the reaction kettle, controlling the temperature to react for 70min, filtering after the reaction is finished, and drying to obtain the bisphenol silyl nano nickel boride.
The antioxidant is bis-cinnamoyl thiodipropionate.
The average molecular weight of the polypropylene is 10 ten thousand.
The average grain diameter of the bisphenol silyl nanometer nickel boride is 0.01 mu m.
The mesh number of the calcium powder is 300 meshes.
The tensile strength of a material sample prepared in the experiment is 8.37MPa, and the elongation at break is 527%; the product has soft touch feeling and smooth and glossy surface, and is similar to silicon rubber.
Example 2
A preparation method of a silica gel-like product material comprises the following components: 25g of SEBS 6151, 52g of paraffin oil, 17g of polypropylene, 2.4g of silicone master batch, 1.2g of antioxidant, 12g of calcium powder and 0.24g of bisphenol silyl nano nickel boride; the preparation scheme is as follows:
adding SEBS 6151, bisphenol silyl nano nickel boride and silicone master batch into a high-speed mixer, slowly adding paraffin oil into the mixer under stirring, controlling the addition to be finished within 80min, continuously stirring for 30min after the addition is finished, standing for 150min after the mixture is uniformly mixed, then adding polypropylene, antioxidant and calcium powder into the mixer, and mixing at high speed for 10min to obtain a mixture; adding the obtained mixture into a double-screw extruder, controlling the rotating speed of a screw to be 130r/min, controlling the feeding speed to be 180r/min, and controlling the temperature to be 190 ℃; and drying the obtained particles at 70 ℃ for 8h, and then performing injection molding to obtain the silica gel imitation product material.
Adding 130g of 0.3mol/L nickel nitrate aqueous solution into a reaction kettle, bubbling with high-purity nitrogen for 8min to remove oxygen, controlling the temperature to be 5 ℃, and protecting with nitrogen; and adding 3.8g of sodium borohydride and 5.4g of sodium hydroxide into 180g of pure water, mixing and stirring uniformly, slowly adding the prepared solution into a reaction kettle, controlling the addition to be finished for 150min, stirring at normal temperature for 3h after the addition is finished, then performing centrifugal filtration, washing and drying to obtain nickel boride nanoparticles, dispersing the obtained nickel boride nanoparticles into 80g of deionized water, then adding 0.3g of methacryloxypropyltrimethoxysilane, heating to 80 ℃, stirring for reaction for 160min, continuing to perform stirring reaction for 50min, cooling to normal temperature, filtering, washing and drying to obtain the modified nano nickel boride.
The preparation method of the bisphenol silyl nano nickel boride comprises the following steps:
adding 24g of modified nano nickel boride, 4g of tetra [ dimethylsiloxane-based ] silane, 5g of diallyl bisphenol and 263g of solvent oil into a reaction kettle, heating to 76 ℃ under the protection of nitrogen, then adding 5g of n-butanol dispersion containing 0.6g of chloroplatinic acid into the reaction kettle, controlling the temperature to react for 120min, filtering after the reaction is finished, and drying to obtain the bisphenol silane based nano nickel boride.
The antioxidant is distearoyl thiodipropionate.
The average molecular weight of the polypropylene is 14 ten thousand.
The average grain diameter of the bisphenol silyl nanometer nickel boride is 0.04 mu m.
The mesh number of the calcium powder is 400 meshes.
The tensile strength of a material sample prepared in the experiment is 8.69MPa, and the elongation at break is 558%; the product has soft touch feeling and smooth and glossy surface, and is similar to silicon rubber.
Example 3
A preparation method of a silica gel-like product material comprises the following components: 30g of SEBS 6151, 56g of paraffin oil, 21g of polypropylene, 3.6g of silicone master batch, 1.8g of antioxidant, 15g of calcium powder and 0.36g of bisphenol silyl nano nickel boride; the preparation scheme is as follows:
adding SEBS 6151, bisphenol silyl nano nickel boride and silicone master batch into a high-speed mixer, slowly adding paraffin oil into the mixer under stirring, controlling the addition to be finished for 90min, continuously stirring for 60min after the addition is finished, standing for 180min after the mixture is uniformly mixed, then adding polypropylene, an antioxidant and calcium powder into the mixer, and mixing at a high speed for 16min to obtain a mixture; adding the obtained mixture into a double-screw extruder, controlling the rotating speed of a screw to be 140r/min, controlling the feeding speed to be 200r/min and controlling the temperature to be 210 ℃; and drying the obtained particles at 80 ℃ for 10h, and then carrying out injection molding to obtain the silica gel imitation product material.
Adding 300g of 1mol/L nickel nitrate aqueous solution into a reaction kettle, carrying out bubbling for 10min by using high-purity nitrogen to remove oxygen, controlling the temperature to 10 ℃, and using nitrogen for protection; in addition, 4.6g of sodium borohydride and 7.2g of sodium hydroxide are added into 200g of pure water, the mixed solution is slowly added into a reaction kettle after being uniformly mixed and stirred, the addition is controlled to be finished within 180min, the solution is stirred for 5h at normal temperature after the completion of the addition, then centrifugal filtration is carried out, nickel boride nanoparticles are obtained after washing and drying, the obtained nickel boride nanoparticles are dispersed into 120g of deionized water, then 0.5g of vinyltrimethoxysilane is added, the temperature is increased to 100 ℃, the stirring reaction is carried out for 180min, the stirring reaction is continuously carried out for 60min, the mixture is cooled to normal temperature, filtered, washed and dried, and then the modified nano nickel boride is obtained.
The preparation method of the bisphenol silyl nano nickel boride comprises the following steps:
adding 35g of modified nano nickel boride, 6g of tetra [ dimethylsiloxy ] silane, 6g of diallyl bisphenol and 300 parts of solvent oil into a reaction kettle, heating to 90 ℃ under the protection of nitrogen, then adding 7g of n-butyl alcohol dispersion containing 0.8g of chloroplatinic acid into the reaction kettle, controlling the temperature to react for 100min, filtering after the reaction is finished, and drying to obtain the bisphenol silyl nano nickel boride.
The antioxidant is dibutyl hydroxy toluene.
The average molecular weight of the polypropylene is 15 ten thousand.
The average grain diameter of the bisphenol silyl nanometer nickel boride is 0.1 mu m.
The mesh number of the calcium powder is 500 meshes.
The tensile strength of a material sample prepared in the experiment is 8.87MPa, and the elongation at break is 561%; the product has soft touch feeling and smooth and glossy surface, and is similar to silicon rubber.
Comparative example 1
A preparation method of a silica gel-like product material comprises the following components: 20g of SEBS 6151, 48g of paraffin oil, 14g of polypropylene, 0.8g of silicone master batch, 0.5g of antioxidant and 8g of calcium powder; the preparation scheme is as follows:
adding SEBS 6151 and silicone master batch into a high-speed mixer, slowly adding paraffin oil into the mixer under stirring, controlling the addition to be finished within 45min, continuously stirring for 10min after the addition is finished, standing for 120min after the mixture is uniformly mixed, then adding polypropylene, antioxidant and calcium powder into the mixer, and mixing at high speed for 8min to obtain a mixture; adding the obtained mixture into a double-screw extruder, controlling the rotating speed of a screw to be 120r/min, controlling the feeding speed to be 160r/min and controlling the temperature to be 185 ℃; and drying the obtained particles at 60 ℃ for 5 hours, and then carrying out injection molding to obtain the silica gel imitation product material.
The antioxidant is bis-cinnamoyl thiodipropionate.
The average molecular weight of the polypropylene is 10 ten thousand.
The mesh number of the calcium powder is 300 meshes.
The tensile strength of a material sample prepared in the experiment is 5.72MPa, and the elongation at break is 442%; the product has soft touch, dull surface and lack of smoothness.
Comparative example 2
Adding 100g of 0.1mol/L nickel nitrate aqueous solution into a reaction kettle, bubbling with high-purity nitrogen for 5min to remove oxygen, controlling the temperature to be 0 ℃, and protecting with nitrogen; in addition, 3.1g of sodium borohydride and 4.5g of sodium hydroxide are added into 150g of pure water, the mixed solution is slowly added into a reaction kettle after being uniformly mixed and stirred, the addition is controlled to be finished within 120min, the solution is stirred for 1h at normal temperature after the addition is finished, then centrifugal filtration is carried out, nickel boride nanoparticles are obtained after washing and drying, the obtained nickel boride nanoparticles are dispersed into 50g of deionized water, then 0.1g of vinyl trimethoxy silane is added, the temperature is increased to 70 ℃, stirring reaction is carried out for 120min, stirring reaction is continued for 180min, the reaction is carried out for 20min, the mixture is cooled to the normal temperature, and then filtration, washing and drying are carried out, thus obtaining the modified nano nickel boride.
The preparation method of the bisphenol silyl nano nickel boride comprises the following steps:
adding 20g of modified nano nickel boride, 1g of tetra [ dimethylsilyloxy alkyl ] silane and 200g of solvent oil into a reaction kettle, heating to 70 ℃ under the protection of nitrogen, then adding 3g of n-butyl alcohol dispersion liquid containing 0.2g of chloroplatinic acid into the reaction kettle, controlling the temperature to react for 70min, filtering after the reaction is finished, and drying to obtain the bisphenol silyl nano nickel boride.
The rest of the process is the same as that of the embodiment 1,
the tensile strength of a material sample prepared in the experiment is 7.61MPa, and the elongation at break is 489%; the product has soft touch, the touch of the product is soft, the surface is dull, and the smoothness is lacked.
Comparative example 3
Adding 100g of 0.1mol/L nickel nitrate aqueous solution into a reaction kettle, bubbling with high-purity nitrogen for 5min to remove oxygen, controlling the temperature to be 0 ℃, and protecting with nitrogen; in addition, 3.1g of sodium borohydride and 4.5g of sodium hydroxide are added into 150g of pure water, the mixed solution is slowly added into a reaction kettle after being uniformly mixed and stirred, the addition is controlled to be finished within 120min, the solution is stirred for 1h at normal temperature after the addition is finished, then centrifugal filtration is carried out, nickel boride nanoparticles are obtained after washing and drying, the obtained nickel boride nanoparticles are dispersed into 50g of deionized water, then 0.1g of vinyl trimethoxy silane is added, the temperature is increased to 70 ℃, stirring reaction is carried out for 120min, stirring reaction is continued for 180min, the reaction is carried out for 20min, the mixture is cooled to the normal temperature, and then filtration, washing and drying are carried out, thus obtaining the modified nano nickel boride.
The preparation method of the bisphenol silyl nano nickel boride comprises the following steps:
adding 20g of modified nano nickel boride, 2g of diallyl bisphenol and 200g of solvent oil into a reaction kettle, heating to 70 ℃ under the protection of nitrogen, then adding 3g of n-butyl alcohol dispersion liquid containing 0.2g of chloroplatinic acid into the reaction kettle, controlling the temperature to react for 70min, filtering after the reaction is finished, and drying to obtain the bisphenol silyl nano nickel boride.
The rest of the process is the same as that of the embodiment 1,
the tensile strength of a material sample prepared in the experiment is 7.02MPa, and the elongation at break is 472%; the product has soft touch, very dull surface and no smooth feeling.

Claims (8)

1. A preparation method of a silica gel-like product material comprises the following components: 20-30 parts of polystyrene-ethylene-butadiene-styrene (SEBS), 48-56 parts of paraffin oil, 14-21 parts of polypropylene, 0.8-3.6 parts of silicone master batch, 0.5-1.8 parts of antioxidant, 8-15 parts of calcium powder and 0.08-0.36 part of bisphenol silyl nano nickel boride; the preparation scheme is as follows:
adding polystyrene-ethylene-butadiene-styrene, bisphenol silyl nano nickel boride and silicone master batch into a high-speed mixer, slowly adding paraffin oil into the mixer under stirring, controlling the addition to be finished within 45-90min, continuing stirring for 10-60min after the addition is finished, standing for 120-180min after uniform mixing, then adding polypropylene, antioxidant and calcium powder into the mixer, and mixing at high speed for 8-16min to obtain a mixture; adding the obtained mixture into a double-screw extruder, controlling the rotating speed of a screw to be 120-; drying the obtained particles at 60-80 ℃ for 5-10h, and then performing injection molding to obtain the silica gel-like product material;
the bisphenol silyl nanometer nickel boride is prepared by performing hydrosilylation reaction on modified nanometer nickel boride, tetra [ dimethylsiloxy ] silane and diallyl bisphenol.
2. The preparation method of the silica gel-like product material according to claim 1, wherein the preparation method of the modified nano nickel boride comprises the following steps:
adding 100-300 parts by mass of 0.1-1mol/L nickel nitrate aqueous solution into a reaction kettle, bubbling with high-purity nitrogen for 5-10min to remove oxygen, controlling the temperature to 0-10 ℃, and protecting with nitrogen; and adding 3.1-4.6 parts of sodium borohydride and 4.5-7.2 parts of sodium hydroxide into 150-200 parts of pure water, mixing and stirring uniformly, slowly adding the prepared solution into a reaction kettle, controlling the addition of the solution for 180min, stirring for 1-5h at normal temperature after completion, then carrying out centrifugal filtration, washing and drying to obtain nickel boride nanoparticles, dispersing the obtained nickel boride nanoparticles into 50-120 parts of deionized water, then adding 0.1-0.5 part of coupling agent, heating to 70-100 ℃, carrying out stirring reaction for 120-180min, continuing stirring and reacting for 20-60min, cooling to normal temperature, filtering, washing, and drying to obtain the modified nano nickel boride.
3. The method for preparing the silica gel-like product material according to claim 3, wherein the bisphenol silyl nano nickel boride is prepared by the following steps:
adding 20-35 parts of modified nano nickel boride, 1-6 parts of tetra [ dimethylsiloxane-based ] silane, 2-6 parts of diallyl bisphenol and 300 parts of solvent oil 200-90 parts by mass into a reaction kettle, heating to 75-90 ℃ under the protection of nitrogen, adding 3-7 parts of n-butyl alcohol dispersion containing 0.2-0.8 part of chloroplatinic acid into the reaction kettle, controlling the temperature to react for 70-100min, filtering after the reaction is finished, and drying to obtain the bisphenol silane-based nano nickel boride.
4. The method of claim 1, wherein the antioxidant is bis-cinnamoylthiobispropionate, bis-stearoylthiobispropionate, or dibutylhydroxytoluene.
5. The method for preparing the material of the imitated silica gel product according to claim 1, wherein the average molecular weight of the polypropylene is 10-15 ten thousand.
6. The method for preparing the silica gel-like product material according to claim 1, wherein the bisphenol silyl nano nickel boride has an average particle size of 0.01 to 0.1 μm.
7. The method for preparing a silica gel-like product material as claimed in claim 1, wherein the mesh size of the calcium powder is 300-500 meshes.
8. The method for preparing the material of claim 1, wherein the coupling agent is one or more selected from vinyltrimethoxysilane and methacryloxypropyltrimethoxysilane.
CN202010541137.3A 2020-06-15 2020-06-15 Preparation method of silica gel-like product material Pending CN111607237A (en)

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Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105295284A (en) * 2015-11-23 2016-02-03 东莞市技塑塑胶科技有限公司 Special material with high resilience for grass of artificial turf and preparation method thereof

Patent Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105295284A (en) * 2015-11-23 2016-02-03 东莞市技塑塑胶科技有限公司 Special material with high resilience for grass of artificial turf and preparation method thereof

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