Elastic floor tile material prepared based on silicone rubber modification and preparation method

Abstract

The invention relates to the technical field of elastic floor tile materials, in particular to an elastic floor tile material prepared based on silicone rubber modification and a preparation method of the elastic floor tile material. Maleic anhydride grafted polypropylene and ethylene propylene rubber serve as main raw materials to prepare an elastomer base material, and a compact cross-linked network structure can be formed in the material; the high-strength elastic base material can effectively resist the impact of external force; in the preparation process of the floor tile material, raw materials and processes which are harmless to human bodies are adopted, so that the floor tile material is soft and comfortable in surface touch feeling, does not cause irritation or harm to skin, and is particularly suitable for places needing to frequently contact with the human bodies; therefore, the elastic floor tile material prepared based on silicone rubber modification has excellent physical and mechanical properties, excellent weather resistance, environmental protection, safety, diversified application scenes and personalized customization capability.

Description

Technical Field

[0001] The invention relates to the technical field of elastic floor tile materials, and in particular to an elastic floor tile material prepared based on silicone rubber modification and a preparation method thereof. Background Art

[0002] In water parks, swimming pools, hot springs, baths, SPAs and other water structures with high safety requirements, elastic floor tiles are often used instead of ceramic tiles. Elastic floor tiles have good resilience, and their comfort and safety are greatly improved. Currently, elastic floor tiles are mostly made of rubber, but due to special application scenarios such as water parks or hot springs, there are higher requirements for the performance of rubber materials, such as water resistance, anti-slip performance, wear resistance, high temperature resistance and corrosion resistance.

[0003] In the prior art, the modification of rubber is mostly carried out by means of material compounding and adding additives, and is only produced through a simple blending process during the preparation process. The performance of the floor tile material prepared in this way is not stable enough, and there is still room for improvement in terms of water resistance, anti-slip performance, wear resistance, high temperature resistance and corrosion resistance. Summary of the invention

[0004] Technical issues solved In view of the above-mentioned shortcomings of the prior art, the present invention provides an elastic floor tile material and a preparation method based on silicone rubber modification, which can effectively solve the problems of poor elasticity, anti-slip properties and weather resistance of the silicone rubber floor tile material in the prior art.

[0005] Technical Solution To achieve the above objectives, the present invention is implemented through the following technical solutions: An elastic floor tile material prepared based on silicone rubber modification, the elastic floor tile material prepared based on silicone rubber modification is composed of the following components: an elastomer substrate, silica-modified silicone rubber, nano-mica, modified graphene oxide and a filler component; The elastomer substrate is made of maleic anhydride grafted polypropylene and ethylene propylene rubber as main raw materials; The silicon dioxide modified silicone rubber is prepared with modified nano silicon dioxide, vinyl-terminated silicone oil, side hydrogen-containing silicone oil, hydrogen-terminated silicone oil and polyvinyl silicone oil as main raw materials; The modified graphene oxide is prepared by surface treating graphene oxide with 1-ethyl-3-methylimidazole dicyandiamide.

[0006] Furthermore, the preparation steps of the elastomer substrate are: Step A, weigh 0.2g of dibenzoyl peroxide and dissolve it in 200g of anhydrous ethanol, stir and dissolve, add 60g of polypropylene and mix evenly, add 2g of maleic anhydride and mix evenly again after ventilation and drying for 24h, and extrude and granulate it through a twin-screw extruder as the first component; Step B, 100g of ethylene-propylene rubber is placed on an open mill, thinned twice and then rolled, then 2g of zinc oxide, 0.5g of stearic acid and 0.3g of stannous chloride dihydrate are added and dispersed evenly, then thinned and rolled into triangle packages three times, and the obtained components are recorded as the second component; Step C, pour the first component and antioxidant 1010 into an internal mixer and mix until completely melted, add the second component and mix for 5 minutes, then add 3g of phenolic resin, dynamically vulcanize for 10 minutes, move to an open mixer to produce sheets, leave it for 24 hours, place it on a flat vulcanizer, preheat, pressurize and cold press to obtain the elastomer substrate.

[0007] Furthermore, the specific operation of stirring and dissolving in step A is stirring at a stirring speed of 500 r / min for 10 min, and the specific operation of mixing evenly in step A is stirring at a stirring speed of 300 r / min for 10 min; in step A, the screw speed of extrusion granulation is 50 r / min, the feed rate is 5 kg / h, and the temperature of extrusion granulation is 140°C for the head, 170°C for the first stage, 180°C for the second stage, 180°C for the third stage, 175°C for the fourth stage, and 160°C for the die.

[0008] Furthermore, the preparation method of the modified nano-silicon dioxide is: 1) Add 0.1g sodium dodecyl sulfate and 3g fumed nano-silica to 100g of 50% ethanol aqueous solution, stir at a stirring speed of 300r / min for 10min, and then ultrasonically disperse at a frequency of 30kHz for 30min, then place in a water bath at 70°C and drop 1g of silane coupling agent KH-570 at a drop rate of 1 drop / s, react at constant temperature for 3h, filter to remove the filtrate, and wash with anhydrous ethanol 3 times, the result is recorded as the pretreatment component; 2) Add the pretreatment component to 80g of 80% ethanol aqueous solution, then add 0.3g of hydroxy silicone oil and 0.1g of dibutyltin dilaurate, stir and react for 5h at a water bath temperature of 25°C and a stirring speed of 100r / min, filter and remove the filtrate, wash it three times with anhydrous ethanol, and then dry it in an oven at 68°C for 2h to obtain modified nano-silica.

[0009] Furthermore, the preparation steps of the silica-modified silicone rubber are: Step i, pour 20g of vinyl-terminated silicone oil, 1.5g of side hydrogen-containing silicone oil, 3g of hydrogen-terminated silicone oil and 1.5g of polyvinyl silicone oil into a flask, stir at a stirring speed of 200r / min for 20min, and record the result as silicone oil component; Step ii, add 1.5g of modified nano-silica to the silicone oil component, stir at a stirring speed of 200r / min for 1h, then add 0.5g of platinum water catalyst, place in a vacuum oven, evacuate and let stand for 6h, and the result is silica-modified silicone rubber.

[0010] Furthermore, the preparation steps of the nano mica are: Step 1, placing the sericite in a muffle furnace at 800°C for activation for 1h, then pouring it into a nitric acid solution with a temperature of 95°C and a concentration of 5mol / L for treatment for 5h, removing the filtrate and washing it with deionized water until neutral, placing it in an oven at 80°C and drying it to constant weight, then pouring it into a saturated sodium chloride solution with a temperature of 80°C for treatment for 3h, removing the filtrate and washing it with deionized water at 80°C for 3 times, and the obtained is recorded as activated mica; Step 2: Pour 2 g of hexadecyltrimethylammonium bromide into 100 g of 80% ethanol aqueous solution, stir to dissolve, heat in a water bath to 80°C, add 10 g of activated mica, ultrasonically treat, and allow to stand for 24 h. Wash three times with deionized water and pour into 100 g of anhydrous ethanol. Ultrasonic crush for 30 min and centrifuge. The lower layer of solid is dried to obtain nano mica.

[0011] Furthermore, the specific operation of stirring and dissolving in step 2 is stirring at a stirring speed of 300 r / min for 10 min, the specific operation of ultrasonic treatment in step 2 is ultrasonic dispersion at a frequency of 30 kHz for 30 min, the power of ultrasonic crushing in step 2 is 200 W, the specific operation of centrifugal treatment in step 2 is centrifugation at a speed of 6000 r / min for 5 min, and the specific operation of drying treatment in step 2 is drying in an oven at 80°C to constant weight.

[0012] Furthermore, the preparation method of the modified graphene oxide is: 1 g of 1-ethyl-3-methylimidazole dicyandiamide, 1 g of potassium hydroxide and 10 g of graphene oxide were poured into 40 g of deionized water, refluxed at 90° C. for 2 h for reaction treatment, then washed with anhydrous ethanol and deionized water three times in sequence, and dried in an oven at 58° C. for 6 h to obtain modified graphene oxide.

[0013] Furthermore, the filler component is prepared by mixing hollow glass microspheres, silicon dioxide powder, basalt fiber, and nano-titanium dioxide in a weight ratio of 3:2:5:1.

[0014] A method for preparing an elastic floor tile material based on silicone rubber modification, the preparation method comprising: Weigh 100 parts by weight of an elastomeric substrate and 30-50 parts by weight of silica-modified silicone rubber, pour them into an internal mixer for melt blending, then add 2-3 parts by weight of nano-mica, 3-4 parts by weight of modified graphene oxide and 2-3 parts by weight of filler components and continue blending for 10 minutes. The result is an elastic floor tile material prepared based on modified silicone rubber.

[0015] Beneficial Effects The present invention provides an elastic floor tile material prepared based on silicone rubber modification and a preparation method. Compared with the prior art, the present invention has the following beneficial effects: 1. The elastomeric substrate prepared with maleic anhydride grafted polypropylene and ethylene propylene rubber as main raw materials in the present invention can form a tight cross-linked network structure inside the material, thereby greatly improving its strength and toughness. This high-strength elastic substrate can effectively resist external impact, ensuring that the floor tiles are not easily damaged during use, thereby extending the service life; due to the use of silicone rubber modification technology, the floor tile material can show excellent elasticity and resilience. Even if it is subjected to pressure or external force for a long time, the floor tile can quickly return to its original state without permanent damage due to deformation. This feature enables the floor tile to provide better comfort and safety under dynamic loads such as walking and running; silicone rubber has excellent water resistance and can effectively prevent moisture from penetrating into the interior of the floor tile. This feature enables the floor tile to maintain its stability and durability in a humid and rainy environment, and will not cause performance degradation or damage due to water absorption and expansion.

[0016] 2. The floor tile material of the present invention can maintain stable performance under extreme temperatures. Whether in high or low temperature environments, the floor tiles can maintain the stability of their physical and chemical properties and will not deform, crack or deteriorate due to temperature changes. This feature makes the floor tiles have broad application prospects in special environments such as outdoor and greenhouses; the addition of nano-mica can significantly improve the wear resistance and scratch resistance of the floor tiles. The nano-mica particles have excellent hardness and wear resistance, can effectively resist scratches and wear from sharp objects, protect the surface of the floor tiles from damage, and maintain a long-lasting bright appearance; components such as nano-titanium dioxide and modified graphene oxide can effectively absorb and scatter ultraviolet rays, reduce the destructive effect of ultraviolet rays on the floor tile materials, and even if exposed to strong sunlight for a long time, the floor tiles can maintain their original color and performance, and will not lose their luster or become fragile due to ultraviolet aging; because the floor tile material has excellent elasticity and surface properties, the floor tiles can still maintain good anti-slip performance in wet or oily conditions. This feature is particularly important for public places, kitchens, bathrooms and other areas that require high anti-slip properties, and can effectively reduce the risk of slipping and falling.

[0017] 3. The addition of modified graphene oxide and nano-mica can give the floor tile material excellent surface properties, so that it has extremely strong anti-fouling ability, is not easy to absorb dust, stains and other impurities, and maintains long-term beauty and cleanliness; the floor tile material of the present invention adopts raw materials and processes that are harmless to the human body during the preparation process, so that the surface feels soft and comfortable, and will not cause irritation or harm to the skin. It is particularly suitable for places that require frequent contact with the human body; therefore, the elastic floor tile material prepared by the present invention based on silicone rubber modification has excellent physical and mechanical properties, excellent weather resistance, environmental protection and safety, as well as diversified application scenarios and personalized customization capabilities. DETAILED DESCRIPTION

[0018] In order to make the purpose, technical solution and advantages of the embodiments of the present invention clearer, the technical solution in the embodiments of the present invention will be clearly and completely described below. Obviously, the described embodiments are part of the embodiments of the present invention, not all of the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without creative work are within the scope of protection of the present invention.

[0019] The present invention will be further described below in conjunction with the embodiments.

[0020] The sources of some components in the embodiments and comparative examples are as follows: Dibenzoyl peroxide, analytical grade, from Guangdong Xilong Chemical Plant; Polypropylene, injection molding grade, Qingdao Shengfule Chemical Co., Ltd.; Maleic anhydride, analytical grade, from Guangdong Xilong Chemical Plant; EPDM, 5045M, Mitsui Chemicals, Japan; Zinc oxide, analytical grade, from Guangdong Xilong Chemical Plant; Stearic acid, analytical grade, from Guangdong Xilong Chemical Plant; Stannous chloride dihydrate, industrial grade, Tianjin Bodi Chemical Co., Ltd.; Antioxidant 1010, industrial grade, Jinjiang Dongxie Chemical Co., Ltd.; Phenolic resin, SP1045, Dongguan Yuebang Rubber Technology Co., Ltd.; Sodium dodecyl sulfate, purity 99%, Xiyi Chemical Shanghai Co., Ltd.; Fumed nano-silica, with a specific surface area of ​​380 m2 / g, from Shanghai Xiyi Chemical Co., Ltd.; Silane coupling agent KH-570, Hangzhou Ruijie Chemical Co., Ltd.; Dibutyltin dilaurate, purity 95%, Xiyi Chemical Shanghai Co., Ltd.; Vinyl-terminated silicone oil, base glue, vinyl content 0.15%, Shanghai Guiyou New Materials Co., Ltd.; Side hydrogenated silicone oil, cross-linking agent, hydrogen content is 0.6%, Shanghai Guiyou New Materials Co., Ltd.; End-hydrogenated silicone oil, cross-linking agent, hydrogen content is 0.15%, Shanghai Tengfei New Materials Co., Ltd.; Polyvinyl silicone oil, catalytic inhibitor and provides more cross-linking sites, vinyl content is 10%, Shanghai Guiyou New Materials Co., Ltd. Platinum water catalyst, Dongguan Wanteng Materials Co., Ltd.; Sericite, Chuzhou Wanqiao Mica Factory; Hexadecyltrimethylammonium bromide, analytical grade, Wuhan Kanosi Technology Co., Ltd.

[0021] Example 1 The elastic floor tile material prepared based on silicone rubber modification of this embodiment is composed of the following components: an elastomer substrate, silica-modified silicone rubber, nano-mica, modified graphene oxide and a filler component; The elastomer substrate is prepared with maleic anhydride grafted polypropylene and ethylene propylene rubber as main raw materials, and the preparation steps are as follows: Step A, weigh 0.2g of dibenzoyl peroxide and dissolve it in 200g of anhydrous ethanol, stir it at a stirring speed of 500r / min for 10min, then add 60g of polypropylene and stir it at a stirring speed of 300r / min for 10min, add 2g of maleic anhydride and mix it again after ventilation and drying for 24h, and record the result after extrusion granulation by a twin-screw extruder as the first component, the screw speed of the extrusion granulation is 50r / min, the feeding amount is 5kg / h, the temperature of the extrusion granulation is 140°C for the head, 170°C for the first stage, 180°C for the second stage, 180°C for the third stage, 175°C for the fourth stage, and 160°C for the die; Step B, 100g of ethylene-propylene rubber is placed on an open mill, thinned twice and then rolled, then 2g of zinc oxide, 0.5g of stearic acid and 0.3g of stannous chloride dihydrate are added and dispersed evenly, then thinned and rolled into triangle packages three times, and the obtained components are recorded as the second component; Step C, pour the first component and antioxidant 1010 into an internal mixer and mix until completely melted, add the second component and mix for 5 minutes, then add 3g of phenolic resin, dynamically vulcanize for 10 minutes, move to an open mixer to produce sheets, leave it for 24 hours, place it on a flat vulcanizer, preheat, pressurize and cold press to obtain the elastomer substrate.

[0022] Silica modified silicone rubber is made from modified nano-silica, vinyl-terminated silicone oil, side hydrogen-containing silicone oil, hydrogen-terminated silicone oil and polyvinyl silicone oil as main raw materials; The preparation method of modified nano silicon dioxide is: 1) Add 0.1g sodium dodecyl sulfate and 3g fumed nano-silica to 100g of 50% ethanol aqueous solution, stir at a stirring speed of 300r / min for 10min, and then ultrasonically disperse at a frequency of 30kHz for 30min, then place in a water bath at 70°C and drop 1g of silane coupling agent KH-570 at a drop rate of 1 drop / s, react at constant temperature for 3h, filter to remove the filtrate, and wash with anhydrous ethanol 3 times, the result is recorded as the pretreatment component; 2) Add the pretreatment component to 80g of 80% ethanol aqueous solution, then add 0.3g of hydroxy silicone oil and 0.1g of dibutyltin dilaurate, stir and react for 5h at a water bath temperature of 25°C and a stirring speed of 100r / min, filter and remove the filtrate, wash it three times with anhydrous ethanol, and then dry it in an oven at 68°C for 2h to obtain modified nano-silica.

[0023] The preparation steps of silica modified silicone rubber are: Step i, pour 20g of vinyl-terminated silicone oil, 1.5g of side hydrogen-containing silicone oil, 3g of hydrogen-terminated silicone oil and 1.5g of polyvinyl silicone oil into a flask, stir at a stirring speed of 200r / min for 20min, and record the result as silicone oil component; Step ii, add 1.5g of modified nano-silica to the silicone oil component, stir at a stirring speed of 200r / min for 1h, then add 0.5g of platinum water catalyst, place in a vacuum oven, evacuate and let stand for 6h, and the result is silica-modified silicone rubber.

[0024] The modified graphene oxide is prepared by surface treating graphene oxide with 1-ethyl-3-methylimidazole dicyandiamide, and the preparation method thereof is as follows: 1 g of 1-ethyl-3-methylimidazole dicyandiamide, 1 g of potassium hydroxide and 10 g of graphene oxide were poured into 40 g of deionized water, refluxed at 90° C. for 2 h for reaction treatment, then washed with anhydrous ethanol and deionized water three times in sequence, and dried in an oven at 58° C. for 6 h to obtain modified graphene oxide.

[0025] The preparation steps of nano mica are: Step 1, placing the sericite in a muffle furnace at 800°C for activation for 1h, then pouring it into a nitric acid solution with a temperature of 95°C and a concentration of 5mol / L for treatment for 5h, removing the filtrate and washing it with deionized water until neutral, placing it in an oven at 80°C and drying it to constant weight, then pouring it into a saturated sodium chloride solution with a temperature of 80°C for treatment for 3h, removing the filtrate and washing it with deionized water at 80°C for 3 times, and the obtained is recorded as activated mica; Step 2, pour 2g of hexadecyltrimethylammonium bromide into 100g of 80% ethanol aqueous solution, stir at a stirring speed of 300r / min for 10min, heat in a water bath to 80°C, add 10g of activated mica, ultrasonically disperse at a frequency of 30kHz for 30min, let stand for 24h, wash with deionized water 3 times, pour into 100g of anhydrous ethanol, ultrasonically crush at a power of 200W for 30min, centrifuge at a speed of 6000r / min for 5min, and dry the lower layer of solid in an oven at 80°C to constant weight to obtain nano mica.

[0026] The filler components are prepared by mixing hollow glass microspheres, silicon dioxide micropowder, basalt fiber and nano titanium dioxide in a weight ratio of 3:2:5:1.

[0027] A method for preparing an elastic floor tile material based on silicone rubber modification, the preparation method comprising: Weigh 100 parts by weight of the elastomer substrate and 30 parts by weight of silica-modified silicone rubber, pour them into an internal mixer for melt blending, then add 2 parts by weight of nano-mica, 3 parts by weight of modified graphene oxide and 2 parts by weight of filler components and continue to blend for 10 minutes. The result is an elastic floor tile material prepared based on modified silicone rubber.

[0028] Example 2 The elastic floor tile material prepared based on silicone rubber modification of this embodiment is composed of the following components: an elastomer substrate, silica-modified silicone rubber, nano-mica, modified graphene oxide and a filler component; The elastomer substrate is prepared with maleic anhydride grafted polypropylene and ethylene propylene rubber as main raw materials, and the preparation steps are as follows: Step A, weigh 0.2g of dibenzoyl peroxide and dissolve it in 200g of anhydrous ethanol, stir it at a stirring speed of 500r / min for 10min, then add 60g of polypropylene and stir it at a stirring speed of 300r / min for 10min, add 2g of maleic anhydride and mix it again after ventilation and drying for 24h, and record the result after extrusion granulation by a twin-screw extruder as the first component, the screw speed of the extrusion granulation is 50r / min, the feeding amount is 5kg / h, the temperature of the extrusion granulation is 140°C for the head, 170°C for the first stage, 180°C for the second stage, 180°C for the third stage, 175°C for the fourth stage, and 160°C for the die; Step B, 100g of ethylene-propylene rubber is placed on an open mill, thinned twice and then rolled, then 2g of zinc oxide, 0.5g of stearic acid and 0.3g of stannous chloride dihydrate are added and dispersed evenly, then thinned and rolled into triangle packages three times, and the obtained components are recorded as the second component; Step C, pour the first component and antioxidant 1010 into an internal mixer and mix until completely melted, add the second component and mix for 5 minutes, then add 3g of phenolic resin, dynamically vulcanize for 10 minutes, move to an open mixer to produce sheets, leave it for 24 hours, place it on a flat vulcanizer, preheat, pressurize and cold press to obtain the elastomer substrate.

[0029] Silica modified silicone rubber is made from modified nano-silica, vinyl-terminated silicone oil, side hydrogen-containing silicone oil, hydrogen-terminated silicone oil and polyvinyl silicone oil as main raw materials; The preparation method of modified nano silicon dioxide is: 1) Add 0.1g sodium dodecyl sulfate and 3g fumed nano-silica to 100g of 50% ethanol aqueous solution, stir at a stirring speed of 300r / min for 10min, and then ultrasonically disperse at a frequency of 30kHz for 30min, then place in a water bath at 70°C and drop 1g of silane coupling agent KH-570 at a drop rate of 1 drop / s, react at constant temperature for 3h, filter to remove the filtrate, and wash with anhydrous ethanol 3 times, the result is recorded as the pretreatment component; 2) Add the pretreatment component to 80g of 80% ethanol aqueous solution, then add 0.3g of hydroxy silicone oil and 0.1g of dibutyltin dilaurate, stir and react for 5h at a water bath temperature of 25°C and a stirring speed of 100r / min, filter and remove the filtrate, wash it three times with anhydrous ethanol, and then dry it in an oven at 68°C for 2h to obtain modified nano-silica.

[0030] The preparation steps of silica modified silicone rubber are: Step i, pour 20g of vinyl-terminated silicone oil, 1.5g of side hydrogen-containing silicone oil, 3g of hydrogen-terminated silicone oil and 1.5g of polyvinyl silicone oil into a flask, stir at a stirring speed of 200r / min for 20min, and record the result as silicone oil component; Step ii, add 1.5g of modified nano-silica to the silicone oil component, stir at a stirring speed of 200r / min for 1h, then add 0.5g of platinum water catalyst, place in a vacuum oven, evacuate and let stand for 6h, and the result is silica-modified silicone rubber.

[0031] The modified graphene oxide is prepared by surface treating graphene oxide with 1-ethyl-3-methylimidazole dicyandiamide, and the preparation method thereof is as follows: 1 g of 1-ethyl-3-methylimidazole dicyandiamide, 1 g of potassium hydroxide and 10 g of graphene oxide were poured into 40 g of deionized water, refluxed at 90° C. for 2 h for reaction treatment, then washed with anhydrous ethanol and deionized water three times in sequence, and dried in an oven at 58° C. for 6 h to obtain modified graphene oxide.

[0032] The preparation steps of nano mica are: Step 1, placing the sericite in a muffle furnace at 800°C for activation for 1h, then pouring it into a nitric acid solution with a temperature of 95°C and a concentration of 5mol / L for treatment for 5h, removing the filtrate and washing it with deionized water until neutral, placing it in an oven at 80°C and drying it to constant weight, then pouring it into a saturated sodium chloride solution with a temperature of 80°C for treatment for 3h, removing the filtrate and washing it with deionized water at 80°C for 3 times, and the obtained is recorded as activated mica; Step 2, pour 2g of hexadecyltrimethylammonium bromide into 100g of 80% ethanol aqueous solution, stir at a stirring speed of 300r / min for 10min, heat in a water bath to 80°C, add 10g of activated mica, ultrasonically disperse at a frequency of 30kHz for 30min, let stand for 24h, wash with deionized water 3 times, pour into 100g of anhydrous ethanol, ultrasonically crush at a power of 200W for 30min, centrifuge at a speed of 6000r / min for 5min, and dry the lower layer of solid in an oven at 80°C to constant weight to obtain nano mica.

[0033] The filler components are prepared by mixing hollow glass microspheres, silicon dioxide micropowder, basalt fiber and nano titanium dioxide in a weight ratio of 3:2:5:1.

[0034] A method for preparing an elastic floor tile material based on silicone rubber modification, the preparation method comprising: Weigh 100 parts by weight of elastomeric substrate and 50 parts by weight of silica-modified silicone rubber, pour them into an internal mixer for melt blending, then add 3 parts by weight of nano-mica, 4 parts by weight of modified graphene oxide and 3 parts by weight of filler components and continue to blend for 10 minutes. The result is an elastic floor tile material prepared based on modified silicone rubber.

[0035] Example 3 The elastic floor tile material prepared based on silicone rubber modification of this embodiment is composed of the following components: an elastomer substrate, silica-modified silicone rubber, nano-mica, modified graphene oxide and a filler component; The elastomer substrate is prepared with maleic anhydride grafted polypropylene and ethylene propylene rubber as main raw materials, and the preparation steps are as follows: Step A, weigh 0.2g of dibenzoyl peroxide and dissolve it in 200g of anhydrous ethanol, stir it at a stirring speed of 500r / min for 10min, then add 60g of polypropylene and stir it at a stirring speed of 300r / min for 10min, add 2g of maleic anhydride and mix it again after ventilation and drying for 24h, and record the result after extrusion granulation by a twin-screw extruder as the first component, the screw speed of the extrusion granulation is 50r / min, the feeding amount is 5kg / h, the temperature of the extrusion granulation is 140°C for the head, 170°C for the first stage, 180°C for the second stage, 180°C for the third stage, 175°C for the fourth stage, and 160°C for the die; Step B, 100g of ethylene-propylene rubber is placed on an open mill, thinned twice and then rolled, then 2g of zinc oxide, 0.5g of stearic acid and 0.3g of stannous chloride dihydrate are added and dispersed evenly, then thinned and rolled into triangle packages three times, and the obtained components are recorded as the second component; Step C, pour the first component and antioxidant 1010 into an internal mixer and mix until completely melted, add the second component and mix for 5 minutes, then add 3g of phenolic resin, dynamically vulcanize for 10 minutes, move to an open mixer to produce sheets, leave it for 24 hours, place it on a flat vulcanizer, preheat, pressurize and cold press to obtain the elastomer substrate.

[0036] Silica modified silicone rubber is made from modified nano-silica, vinyl-terminated silicone oil, side hydrogen-containing silicone oil, hydrogen-terminated silicone oil and polyvinyl silicone oil as main raw materials; The preparation method of modified nano silicon dioxide is: 1) Add 0.1g sodium dodecyl sulfate and 3g fumed nano-silica to 100g of 50% ethanol aqueous solution, stir at a stirring speed of 300r / min for 10min, and then ultrasonically disperse at a frequency of 30kHz for 30min, then place in a water bath at 70°C and drop 1g of silane coupling agent KH-570 at a drop rate of 1 drop / s, react at constant temperature for 3h, filter to remove the filtrate, and wash with anhydrous ethanol 3 times, the result is recorded as the pretreatment component; 2) Add the pretreatment component to 80g of 80% ethanol aqueous solution, then add 0.3g of hydroxy silicone oil and 0.1g of dibutyltin dilaurate, stir and react for 5h at a water bath temperature of 25°C and a stirring speed of 100r / min, filter and remove the filtrate, wash it three times with anhydrous ethanol, and then dry it in an oven at 68°C for 2h to obtain modified nano-silica.

[0037] The preparation steps of silica modified silicone rubber are: Step i, pour 20g of vinyl-terminated silicone oil, 1.5g of side hydrogen-containing silicone oil, 3g of hydrogen-terminated silicone oil and 1.5g of polyvinyl silicone oil into a flask, stir at a stirring speed of 200r / min for 20min, and record the result as silicone oil component; Step ii, add 1.5g of modified nano-silica to the silicone oil component, stir at a stirring speed of 200r / min for 1h, then add 0.5g of platinum water catalyst, place in a vacuum oven, evacuate and let stand for 6h, and the result is silica-modified silicone rubber.

[0038] The modified graphene oxide is prepared by surface treating graphene oxide with 1-ethyl-3-methylimidazole dicyandiamide, and the preparation method thereof is as follows: 1 g of 1-ethyl-3-methylimidazole dicyandiamide, 1 g of potassium hydroxide and 10 g of graphene oxide were poured into 40 g of deionized water, refluxed at 90° C. for 2 h for reaction treatment, then washed with anhydrous ethanol and deionized water three times in sequence, and dried in an oven at 58° C. for 6 h to obtain modified graphene oxide.

[0039] The preparation steps of nano mica are: Step 1, placing the sericite in a muffle furnace at 800°C for activation for 1h, then pouring it into a nitric acid solution with a temperature of 95°C and a concentration of 5mol / L for treatment for 5h, removing the filtrate and washing it with deionized water until neutral, placing it in an oven at 80°C and drying it to constant weight, then pouring it into a saturated sodium chloride solution with a temperature of 80°C for treatment for 3h, removing the filtrate and washing it with deionized water at 80°C for 3 times, and the obtained is recorded as activated mica; Step 2, pour 2g of hexadecyltrimethylammonium bromide into 100g of 80% ethanol aqueous solution, stir at a stirring speed of 300r / min for 10min, heat in a water bath to 80°C, add 10g of activated mica, ultrasonically disperse at a frequency of 30kHz for 30min, let stand for 24h, wash with deionized water 3 times, pour into 100g of anhydrous ethanol, ultrasonically crush at a power of 200W for 30min, centrifuge at a speed of 6000r / min for 5min, and dry the lower layer of solid in an oven at 80°C to constant weight to obtain nano mica.

[0040] The filler components are prepared by mixing hollow glass microspheres, silicon dioxide micropowder, basalt fiber and nano titanium dioxide in a weight ratio of 3:2:5:1.

[0041] A method for preparing an elastic floor tile material based on silicone rubber modification, the preparation method comprising: Weigh 100 parts by weight of elastomeric substrate and 40 parts by weight of silica-modified silicone rubber, pour them into an internal mixer for melt blending, then add 3 parts by weight of nano-mica, 3 parts by weight of modified graphene oxide and 3 parts by weight of filler components and continue blending for 10 minutes. The result is an elastic floor tile material prepared based on modified silicone rubber.

[0042] Comparative Example 1 The elastic floor tile material and preparation method based on silicone rubber modification provided in this comparative example are substantially the same as those in Example 1, with the main difference being that in this comparative example 1, the elastomer substrate in Example 1 is replaced with a thermoplastic elastomer of model number Hytrel-4058.

[0043] Comparative Example 2 The elastic floor tile material and preparation method based on silicone rubber modification provided in this comparative example are roughly the same as those in Example 1, with the main difference being that in this comparative example 2, the silica-modified silicone rubber in Example 1 is replaced with a thermoplastic elastomer of model 703.

[0044] Comparative Example 3 The elastic floor tile material and preparation method based on silicone rubber modification provided in this comparative example are substantially the same as those in Example 1, with the main difference being that in this comparative example 3, the modified graphene oxide in Example 1 is replaced with unmodified graphene oxide.

[0045] Performance Testing The elastic floor tile materials based on silicone rubber modification prepared in Examples 1-3 and Comparative Examples 1-3 are marked as Example 1, Example 2, Example 3, Comparative Example 1, Comparative Example 2 and Comparative Example 3, respectively. Then, the performance of Examples 1-3 and Comparative Examples 1-3 is tested. The specific testing methods and test items are as follows: 1. The tensile strength and elongation at break of Examples 1-3 and Comparative Examples 1-3 were tested according to the standard of GB / T528-1998, and the obtained data are recorded in the following table; 2. The tear strength of Examples 1-3 and Comparative Examples 1-3 was tested with reference to the standard of GB / T529-2008, with a tear rate of 500 mm / min. The obtained data are recorded in the following table; 3. Referring to the standard of GB / T23651-2009, the tear strength of Examples 1-3 and Comparative Examples 1-3 was tested using LX-A rubber hardness tester Shore A hardness, with a tear rate of 500 mm / min. The obtained data are recorded in the following table;

[0046] It can be seen from the data in the above table that the mechanical properties such as tensile strength of the elastic floor tile materials prepared based on silicone rubber modification in Examples 1-3 are significantly better than those in Comparative Examples 1-3, indicating that adding an elastomeric substrate, silica-modified silicone rubber and modified graphene oxide in the process of preparing the elastic floor tile materials prepared based on silicone rubber modification can improve the material properties.

[0047] It should be noted that, in this article, relational terms such as first and second, etc. are only used to distinguish one entity or operation from another entity or operation, and do not necessarily require or imply any such actual relationship or order between these entities or operations. Moreover, the terms "include", "comprise" or any other variants thereof are intended to cover non-exclusive inclusion, so that a process, method, article or device including a series of elements includes not only those elements, but also other elements not explicitly listed, or also includes elements inherent to such process, method, article or device. In the absence of further restrictions, the elements defined by the sentence "comprise a ..." do not exclude the existence of other identical elements in the process, method, article or device including the elements.

[0048] The above embodiments are only used to illustrate the technical solutions of the present invention, rather than to limit the same. Although the present invention has been described in detail with reference to the aforementioned embodiments, those skilled in the art should understand that the technical solutions described in the aforementioned embodiments may still be modified, or some of the technical features may be replaced by equivalents. Such modifications or replacements will not cause the essence of the corresponding technical solutions to deviate from the spirit and scope of the technical solutions of the embodiments of the present invention.

Claims

1. An elastic floor tile material prepared based on silicone rubber modification, characterized in that: The elastic floor tile material prepared based on silicone rubber modification is composed of the following components: an elastomer substrate, silica-modified silicone rubber, nano-mica, modified graphene oxide and a filler component; The elastomer substrate is made of maleic anhydride grafted polypropylene and ethylene propylene rubber as main raw materials; The silicon dioxide modified silicone rubber is prepared with modified nano silicon dioxide, vinyl-terminated silicone oil, side hydrogen-containing silicone oil, hydrogen-terminated silicone oil and polyvinyl silicone oil as main raw materials; The modified graphene oxide is prepared by surface treating graphene oxide with 1-ethyl-3-methylimidazole dicyandiamide.

2. The elastic floor tile material prepared based on silicone rubber modification according to claim 1, characterized in that: The preparation steps of the elastomer substrate are: Step A, weigh 0.2g of dibenzoyl peroxide and dissolve it in 200g of anhydrous ethanol, stir and dissolve, add 60g of polypropylene and mix evenly, add 2g of maleic anhydride and mix evenly again after ventilation and drying for 24h, and extrude and granulate it through a twin-screw extruder as the first component; Step B, 100g of ethylene-propylene rubber is placed on an open mill, thinned twice and then rolled, then 2g of zinc oxide, 0.5g of stearic acid and 0.3g of stannous chloride dihydrate are added and dispersed evenly, then thinned and rolled into triangle packages three times, and the obtained components are recorded as the second component; Step C, pour the first component and antioxidant 1010 into an internal mixer and mix until completely melted, add the second component and mix for 5 minutes, then add 3g of phenolic resin, dynamically vulcanize for 10 minutes, move to an open mixer to produce sheets, leave it for 24 hours, place it on a flat vulcanizer, preheat, pressurize and cold press to obtain the elastomer substrate.

3. The elastic floor tile material prepared based on silicone rubber modification according to claim 2, characterized in that: The specific operation of stirring and dissolving in step A is stirring at a stirring speed of 500 r / min for 10 min, and the specific operation of mixing evenly in step A is stirring at a stirring speed of 300 r / min for 10 min.

4. The elastic floor tile material prepared based on silicone rubber modification according to claim 1, characterized in that: The preparation method of the modified nano silicon dioxide is: 1) Add 0.1g sodium dodecyl sulfate and 3g fumed nano-silica to 100g of 50% ethanol aqueous solution, stir at a stirring speed of 300r / min for 10min, and then ultrasonically disperse at a frequency of 30kHz for 30min, then place in a water bath at 70°C and drop 1g of silane coupling agent KH-570 at a drop rate of 1 drop / s, react at constant temperature for 3h, filter to remove the filtrate, and wash with anhydrous ethanol 3 times, the result is recorded as the pretreatment component; 2) Add the pretreatment component to 80g of 80% ethanol aqueous solution, then add 0.3g of hydroxy silicone oil and 0.1g of dibutyltin dilaurate, stir and react for 5h at a water bath temperature of 25°C and a stirring speed of 100r / min, filter and remove the filtrate, wash it three times with anhydrous ethanol, and then dry it in an oven at 68°C for 2h to obtain modified nano-silica.

5. The elastic floor tile material prepared based on silicone rubber modification according to claim 1, characterized in that: The preparation steps of the silicon dioxide modified silicone rubber are: Step i, pour 20g of vinyl-terminated silicone oil, 1.5g of side hydrogen-containing silicone oil, 3g of hydrogen-terminated silicone oil and 1.5g of polyvinyl silicone oil into a flask, stir at a stirring speed of 200r / min for 20min, and record the result as silicone oil component; Step ii, add 1.5g of modified nano-silica to the silicone oil component, stir at a stirring speed of 200r / min for 1h, then add 0.5g of platinum water catalyst, place in a vacuum oven, evacuate and let stand for 6h, and the result is silica-modified silicone rubber.

6. The elastic floor tile material prepared based on silicone rubber modification according to claim 1, characterized in that: The preparation steps of the nano mica are: Step 1, placing the sericite in a muffle furnace at 800°C for activation for 1h, then pouring it into a nitric acid solution with a temperature of 95°C and a concentration of 5mol / L for treatment for 5h, removing the filtrate and washing it with deionized water until neutral, placing it in an oven at 80°C and drying it to constant weight, then pouring it into a saturated sodium chloride solution with a temperature of 80°C for treatment for 3h, removing the filtrate and washing it with deionized water at 80°C for 3 times, and the obtained is recorded as activated mica; Step 2: Pour 2 g of hexadecyltrimethylammonium bromide into 100 g of 80% ethanol aqueous solution, stir to dissolve, heat in a water bath to 80°C, add 10 g of activated mica, ultrasonically treat, and allow to stand for 24 h. Wash three times with deionized water and pour into 100 g of anhydrous ethanol. Ultrasonic crush for 30 min and centrifuge. The lower layer of solid is dried to obtain nano mica.

7. The elastic floor tile material prepared based on silicone rubber modification according to claim 6, characterized in that: The specific operation of stirring and dissolving in step 2 is stirring at a stirring speed of 300 r / min for 10 min, the specific operation of ultrasonic treatment in step 2 is ultrasonic dispersion at a frequency of 30 kHz for 30 min, the power of ultrasonic crushing in step 2 is 200 W, the specific operation of centrifugal treatment in step 2 is centrifugation at a speed of 6000 r / min for 5 min, and the specific operation of drying treatment in step 2 is drying in an oven at 80°C to constant weight.

8. The elastic floor tile material prepared based on silicone rubber modification according to claim 1, characterized in that: The preparation method of the modified graphene oxide is: 1 g of 1-ethyl-3-methylimidazole dicyandiamide, 1 g of potassium hydroxide and 10 g of graphene oxide were poured into 40 g of deionized water, refluxed at 90° C. for 2 h for reaction treatment, then washed with anhydrous ethanol and deionized water three times in sequence, and dried in an oven at 58° C. for 6 h to obtain modified graphene oxide.

9. The elastic floor tile material prepared based on silicone rubber modification according to claim 1, characterized in that: The filler component is prepared by mixing hollow glass microspheres, silicon dioxide powder, basalt fiber and nano titanium dioxide in a weight ratio of 3:2:5:

1.

10. A method for preparing an elastic floor tile material based on silicone rubber modification according to any one of claims 1 to 9, characterized in that: The preparation method is: Weigh 100 parts by weight of an elastomeric substrate and 30-50 parts by weight of silica-modified silicone rubber, pour them into an internal mixer for melt blending, then add 2-3 parts by weight of nano-mica, 3-4 parts by weight of modified graphene oxide and 2-3 parts by weight of filler components and continue blending for 10 minutes. The result is an elastic floor tile material prepared based on modified silicone rubber.

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