CN113717475A - Rubber floor raw material composition, rubber floor and preparation method and application thereof - Google Patents
Rubber floor raw material composition, rubber floor and preparation method and application thereof Download PDFInfo
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- CN113717475A CN113717475A CN202111062507.6A CN202111062507A CN113717475A CN 113717475 A CN113717475 A CN 113717475A CN 202111062507 A CN202111062507 A CN 202111062507A CN 113717475 A CN113717475 A CN 113717475A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L23/00—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers
- C08L23/02—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers not modified by chemical after-treatment
- C08L23/16—Elastomeric ethene-propene or ethene-propene-diene copolymers, e.g. EPR and EPDM rubbers
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B61—RAILWAYS
- B61D—BODY DETAILS OR KINDS OF RAILWAY VEHICLES
- B61D17/00—Construction details of vehicle bodies
- B61D17/04—Construction details of vehicle bodies with bodies of metal; with composite, e.g. metal and wood body structures
- B61D17/10—Floors
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B62—LAND VEHICLES FOR TRAVELLING OTHERWISE THAN ON RAILS
- B62D—MOTOR VEHICLES; TRAILERS
- B62D25/00—Superstructure or monocoque structure sub-units; Parts or details thereof not otherwise provided for
- B62D25/20—Floors or bottom sub-units
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B62—LAND VEHICLES FOR TRAVELLING OTHERWISE THAN ON RAILS
- B62D—MOTOR VEHICLES; TRAILERS
- B62D29/00—Superstructures, understructures, or sub-units thereof, characterised by the material thereof
- B62D29/04—Superstructures, understructures, or sub-units thereof, characterised by the material thereof predominantly of synthetic material
- B62D29/043—Superstructures
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- E—FIXED CONSTRUCTIONS
- E04—BUILDING
- E04F—FINISHING WORK ON BUILDINGS, e.g. STAIRS, FLOORS
- E04F15/00—Flooring
- E04F15/02—Flooring or floor layers composed of a number of similar elements
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- E—FIXED CONSTRUCTIONS
- E04—BUILDING
- E04F—FINISHING WORK ON BUILDINGS, e.g. STAIRS, FLOORS
- E04F15/00—Flooring
- E04F15/18—Separately-laid insulating layers; Other additional insulating measures; Floating floors
- E04F15/181—Insulating layers integrally formed with the flooring or the flooring elements
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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
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- C08K2003/2227—Oxides; Hydroxides of metals of aluminium
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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
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- C08K2003/2296—Oxides; Hydroxides of metals of zinc
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- C08L2201/00—Properties
- C08L2201/02—Flame or fire retardant/resistant
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- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02T—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO TRANSPORTATION
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Abstract
The invention provides a rubber floor raw material composition, a rubber floor, a preparation method and an application thereof. The rubber floor raw material composition comprises: ethylene propylene diene monomer, silicone rubber, EVA resin, zinc oxide, stearic acid, oxidized polyethylene wax, erucamide, polyethylene wax, polyethylene glycol, hydrophobic group modified aluminum hydroxide, hydrophobic group modified white carbon black and vulcanizing agent. The invention also provides a rubber floor obtained from the rubber floor raw material composition and a preparation method of the rubber floor. The invention further provides application of the rubber floor in vehicles and architectural decoration. The rubber floor has high hydrophobicity and good self-cleaning capability, does not need to be waxed in the using process, and is low in maintenance cost.
Description
Technical Field
The invention relates to the technical field of building decoration materials, in particular to a self-cleaning and easy-to-clean rubber floor raw material composition, a rubber floor and a preparation method and application thereof.
Background
The rubber floor is an elastic floor material which is widely applied, and is widely applied to various public places due to the characteristics of strong elasticity, sound insulation, skid resistance, waterproofness and the like.
The rubber is a high-elasticity polymer material with reversible deformation, has strong elasticity at room temperature, and is easy to be corroded by stains and further form dirt because the surface structure of the rubber is loose and the compactness is not strong, so that the surface of the rubber is difficult to clean. Specifically, the following problems currently exist with the rubber flooring on the market:
1. at present, the surface of the rubber floor is waxed to form a hardened isolation layer on the surface of the rubber floor cloth, so that the problem of poor stain resistance of the surface of the rubber floor is solved, but the surface of the rubber floor is waxed only to have a certain effect in a short time;
2. the scratch resistance of the surface of the rubber floor is reduced after waxing, and white marks can be left after the rubber floor is scratched by relatively hard objects, so that the decorative attractiveness of the rubber floor is seriously influenced;
3. no matter the wood floor is a rubber floor or a household wood floor, the surface waxing needs professional personnel to operate, the difficulty is increased for daily maintenance, and meanwhile, the maintenance cost of the whole life cycle of the product is increased.
According to the standard requirements of rubber floor (cloth) in different industries, the related technical standards mainly comprise:
conventional physical and mechanical properties: in order to ensure that the product has normal use capability in the life cycle;
fireproof performance: the fire-proof device meets the fire-proof requirements of different industries, prevents the fire accident from occurring, ensures that no harmful substance is generated or not during burning, prevents flame from spreading, does not generate dense smoke, and further prolongs the time and probability of escaping and rescuing.
The rubber floor (cloth) is used as one of floor decoration materials, the aesthetic property of the product is one of very important characteristics, besides the product meets the conventional physical and mechanical properties, fire resistance and environmental protection performance, the stain resistance (easy cleaning property) of the product plays a very important role in the application of the product, in different industry standards of the current rubber floor (cloth), the requirement on the stain resistance is mainly measured by different solvent/solution resistance, and the actual trampling experiment and other experiment standards of the product are relatively few.
Similar hydrophobic self-cleaning use technology and related technical patents and documents are not inquired in the rubber floor (cloth) or elastic floor industry products at present.
Disclosure of Invention
In order to solve the problems, the invention aims to provide a rubber floor raw material composition, a rubber floor, and a preparation method and application thereof. The rubber floor has high hydrophobicity and good self-cleaning capability, does not need to be waxed in the using process, and is low in maintenance cost.
In order to achieve the purpose, the invention provides a rubber floor raw material composition which comprises, by weight, 50-80 parts of ethylene propylene diene monomer, 5-25 parts of silicone rubber, 5-25 parts of EVA resin, 3-8 parts of zinc oxide, 0.5-3 parts of stearic acid, 1-7 parts of oxidized polyethylene wax, 0.4-2.2 parts of erucamide, 0.3-4 parts of polyethylene wax, 0.5-2.5 parts of polyethylene glycol, 100 parts of hydrophobic modified aluminum hydroxide, 15-40 parts of hydrophobic modified white carbon black and 1.5-6 parts of vulcanizing agent.
According to the invention, the raw material composition of the rubber floor is formed by adding the silicon rubber, the ethylene propylene diene monomer rubber and the EVA resin as main materials, the polyethylene wax, the oxidized polyethylene wax and the erucamide as high-molecular protective materials and the hydrophobic group material, so that the prepared rubber floor can meet the requirements of mechanical property, low-smoke fireproof performance and halogen-free environment-friendly performance of an industrial standard floor, and can obtain the floor surface with a hydrophobic hardened layer, thereby achieving the effects of isolating from stains and self-cleaning. In some embodiments, the rubber floor may be a rubber floor block or a rubber floor cloth.
In a specific embodiment of the present invention, preferably, the ethylene propylene diene monomer, the silicone rubber, and the EVA resin (ethylene-vinyl acetate copolymer) are used as a main material, the weight ratio of the silicone rubber in the main material is 18-36% (e.g., 20%, 25%, 30%, 35%, etc.), the weight ratio of the ethylene propylene diene monomer in the main material is 40-80% (e.g., 50%, 60%, 70%, etc.), and the weight ratio of the EVA in the main material is 12-30%, e.g., 15-20%. The weight proportion of the main material in the rubber floor material composition is generally controlled to be 24-55%. In some embodiments, the total weight parts of the host material may be controlled to be 100 parts.
In a particular embodiment of the invention, the ethylene propylene diene monomer may comprise ethylene propylene diene monomer of the dow chemical EPDM4570 type.
In a particular embodiment of the present invention, the silicone rubber may include methyl vinyl silicone rubber.
In particular embodiments of the invention, the EVA resin may include EVA18, i.e. EVA18 series products, such as EVA18-3, EVA18J3, etc. produced by the Yanshan petrochemical industry.
In a particular embodiment of the invention, the polyethylene wax, oxidized polyethylene wax and erucamide are the repellent materials. When the raw material composition is used for preparing the floor, the oxidized polyethylene wax forms the outermost layer of the floor, and plays the roles of isolating stains and self-cleaning. The polyethylene wax forms a secondary outer layer surface, is used for increasing the bonding strength between the oxidized polyethylene wax and the main body material, and can also increase the surface hardness of the rubber floor. In a specific embodiment, the polyethylene wax may be selected from polyethylene wax 1040P. The polyethylene wax is typically present in an amount of from 1 to 5% by weight of the total weight of the rubber flooring material composition. The total weight of the polyethylene wax and the erucamide is generally 0.5-2% of the total weight of the rubber floor raw material composition, so as to avoid precipitation on the surface of the rubber floor.
In a particular embodiment of the invention, the oxidized polyethylene wax comprises OPE90 and the like.
In the specific embodiment of the invention, the erucamide comprises erucamide with 90% of erucic acid content in the raw material, the purity of the finished product of the erucamide is high, and the content of the erucamide can reach more than 98%.
In a specific embodiment of the invention, the hydrophobic group modified aluminum hydroxide and the hydrophobic agent modified white carbon black have the functions of fire prevention and reinforcement.
In particular embodiments of the present invention, the vulcanizing agent may be present in an amount of 1.5 to 5 parts by weight, 1.5 to 4 parts by weight, and the like. The curing agent may include a peroxide curing agent and/or a curing co-agent.
In a specific embodiment of the present invention, the polyethylene glycol may include polyethylene glycol 6000, and the like.
In a particular embodiment of the invention, the zinc oxide may comprise nano zinc oxide, preferably having a particle size of 10-100 μm, for example 50 μm.
The invention also provides a rubber floor which is prepared from the rubber floor raw material composition.
The invention also provides a preparation method of the rubber floor, which comprises the following steps: and sequentially carrying out first-stage banburying, second-stage banburying, extrusion calendering, vulcanization edge cutting and polishing on the rubber floor raw material composition to obtain the rubber floor.
In the above preparation method, preferably, in the first banburying step, the temperature of the first banburying is 60-160 ℃ (e.g. 60-130 ℃, 90-160 ℃), the pressure of the first banburying is 10-55kg (e.g. 10-45kg, 20-45kg), the rotation speed of the rotor is 20-50r/min (e.g. 40-50r/min), and the time of the first banburying is 90s-150 s. The temperature of the first banburying and dumping is generally above 140 ℃, for example above 150 ℃ so as to enable the oxidized polyethylene wax to be fully melted. In the first banburying process, the oxidized polyethylene wax begins to melt at the temperature of 95-100 ℃, and the polyethylene wax can play a role in lubricating the internal structure of the rubber, improve the compatibility between the rubber and other raw materials and well disperse the rubber in the raw materials; when the temperature reaches 140-150 ℃, the oxidized polyethylene wax begins to melt and then forms a layer of hardened wax film on the surface of the rubber matrix.
In some embodiments, the above preparation method may be a first banburying step after mixing the subject materials subjected to banburying in advance with other raw material compositions which are not banburied. The conditions under which the host material is subjected to prior banburying are generally: the mixing temperature is 40-90 deg.C (e.g. 60-90 deg.C), the mixing pressure is generally 15-50kg (e.g. 20-40kg), the rotor speed is generally 30-50, and the mixing time is generally controlled to 60-80 s.
In the above preparation method, preferably, in the second banburying step, the temperature of the second banburying is 70-110 ℃, the pressure of the second banburying is 10-55kg (for example, 20-50kg), the rotation speed of a rotor is 15-50r/min, the time of the second banburying is 90s-150s, and the dumping temperature of the second banburying is 70-120 ℃.
In the above production method, preferably, in the step of extrusion calendering, the temperature of the head of the extruder is 45 to 95 ℃ (e.g., 45 to 85 ℃, 55 to 95 ℃), the temperature of the body is 45 to 95 ℃ (e.g., 45 to 85 ℃), the rotation speed of the screw of the extruder is 5 to 15r/min, and the temperature of the calender roll is 45 to 80 ℃.
In the above-mentioned preparation method, in the step of vulcanizing the cut edge, the vulcanization temperature is generally controlled to (150-. In view of economic efficiency, a vulcanization temperature of 180 ℃ may be generally selected. The vulcanization pressure is generally (3.0-5.5). + -. 0.3kg/cm2The effective vulcanization time is (4-20) + -0.1 min, and the cutting edge width is 1218 + -1 mm.
The invention further provides the application of the rubber floor in vehicles. In particular, the vehicles include, but are not limited to, rail vehicles, ground buses, ships, and the like. The rail transit vehicles can include, but are not limited to, railway motor train units, common passenger trains, light rail vehicles, trams, subway vehicles, urban rails, maglev vehicles, and the like.
The invention also provides the application of the rubber floor in building decoration. Specifically, the buildings include, but are not limited to, libraries, museums, hospitals, airports, kindergartens, mini-computer rooms, gymnasiums, geriatric homes, sporting events, office buildings, industrial plants, and the like.
Compared with the prior rubber floor (cloth) technology, the self-cleaning rubber floor for the floor covering and paving material of the ground covering has the following advantages:
1. the rubber floor provided by the invention meets various technical standards of the rubber floor (cloth) industry, has obvious fireproof performance advantages, wherein the smoke density is less than 50 (the technical standard requirement of the civil building industry is less than 500, and the technical standard requirement of the railway industry is less than 200), and the combustion safety of the product is improved.
2. According to the preparation method of the rubber floor provided by the invention, through reasonably blending the formula, the prepared rubber floor has the functions of self cleaning and easy cleaning, the difficulty that the product is difficult to clean in the using process is solved, waxing is avoided in the using process of the floor, the maintenance cost of the whole life cycle of the product is reduced, and the beautiful effect of keeping bright color in the using process of the product is improved.
Detailed Description
The technical solutions of the present invention will be described in detail below in order to clearly understand the technical features, objects, and advantages of the present invention, but the present invention is not limited to the practical scope of the present invention.
The experimental methods in the following examples are all conventional methods, and the various raw materials used in the following examples, except for the modified materials, are all commercially available materials. Wherein:
the ethylene propylene diene monomer is Dow chemical EPDM 4570;
the silicon rubber is methyl vinyl silicon rubber;
the EVA resin is EVA resin 18;
the vulcanizing agent is peroxide vulcanizing agent, and the manufacturer is Achima chemical Co., Ltd;
the white carbon black is hydrophobic base material modified white carbon black (hereinafter referred to as modified white carbon black), and the manufacturer is New dilute metallurgy chemical industry Co., Ltd, Guangzhou;
aluminum hydroxide is modified aluminum hydroxide (hereinafter referred to as modified aluminum hydroxide) as a hydrophobic group, and the manufacturer is Zibowan New materials Co., Ltd;
the zinc oxide is nano zinc oxide PZT-15 with the grain diameter of 10-100 μm, and the manufacturer is Nanjing Baokite new material Co., Ltd;
stearic acid, polyethylene wax, polyethylene glycol 6000, erucamide, oleamide, oxidized polyethylene wax are OPE90 and are conventionally sold in the market.
The test items referred to below are performed with reference to national standards or industries, wherein,
hardness reference GB/T531.1 "vulcanized rubber or thermoplastic rubber indentation hardness test method part 1: shore Durometer method (Shore hardness), test method.
The strength is determined according to a test method of GB/T528 'determination of tensile stress strain performance of vulcanized rubber or thermoplastic rubber'.
The tear strength is determined by test methods in GB/T529 test methods for the determination of the tear strength of vulcanized rubber or thermoplastic rubber (trouser, right-angled and crescent test specimens).
The elongation at break refers to the test method of GB/T528 'determination of tensile stress strain performance of vulcanized rubber or thermoplastic rubber'.
The contact angle of the water drop is referred to GB/T24368 glass surface hydrophobic contaminant detection contact angle measurement method. Contact angles < 90 ° are generally referred to as non-hydrophobic (hydrophilic), contact angles > 90 ° as hydrophobic, and contact angles > 150 ° as superhydrophobic.
The oxygen index is referred to GB/T2406.2 plastics, the combustion behaviour is determined by the oxygen index method part 2: room Temperature Test (RTT) test method.
The smoke density is referred to GB/T8323.2 plastic smoke generation part 2: test method of single chamber method for measuring smoke density.
TVOC refers to ISO 12219-2 interfacial air of road vehicles-Part 2 Screening method for the determination of the emission of floor organic compounds from floor vehicles and materials-Bag method test method.
The anti-slip rating is referred to DIN 51130 test method "floor anti-slip test".
The solvent resistance is determined according to ISO 26987 Standard test methods "Resilience floor coverage-Determination of standing and resistance to chemicals".
The coffee resistance, the tea stain resistance, the oil resistance pen and the water resistance pen are all visually observed by people according to an experimental method of HG/T3828-2006 indoor water-based woodware paint.
Experimental group 1
Comparative examples 1 to 5 provide rubber floor material compositions different in the kind of the material of the main body. Table 1 shows the compositions in parts by weight of the rubber floor material compositions of comparative examples 1 to 5.
TABLE 1
Preparing the rubber floor raw material composition in each proportion into a rubber floor (specifically, a floor block or floor cloth) according to the following method:
I. first stage internal mixing
One or more than two of the ethylene propylene diene monomer rubber, the EVA resin and the silicon rubber are put into an internal mixer, the internal mixing temperature is 40-90 ℃, the internal mixing pressure is 15-50kg, the rotor speed is 15-25r/min, and the internal mixing is carried out for 60-80 s; then adding the modified white carbon black, the nano zinc oxide, the stearic acid and the polyethylene glycol in sequence, wherein the banburying temperature is 60-130 ℃, the banburying pressure is 10-45kg, the rotor speed is 20-50r/min, the banburying is 90-150s, the banburying and rubber discharging temperature is 150-160 ℃, and the sheet discharging, cooling and standing are carried out for at least more than 4 hours;
II, second-stage banburying
Putting the materials subjected to banburying in the step I into a banbury mixer according to parts by weight, adding a vulcanizing agent, banburying at 70-110 ℃, banburying pressure within (10-50) kg, rotor rotating speed within (15-50) r/min, banburying for 90-150s, banburying rubber-removing temperature within 70-120 ℃, sheet-discharging, cooling and standing for at least more than 8 hours;
extrusion calendering III
Extruding the material in the step II into a rubber sheet by a cold-feeding wide extruder, wherein the temperature of a machine head of the extruder is (45-95) DEG C, the temperature of a machine body is as follows: (45-85) DEG C, the rotating speed of a screw of the extruder is 5-15r/min, the temperature of a calendering roller is (35-80) DEG C, and the rubber sheet is parked for at least 4 hours;
IV, vulcanizing and cutting edges
Vulcanizing and molding the film extruded in the step III on a drum vulcanizer, and simultaneously performing online trimming of two-side flash, wherein the control range of the vulcanization temperature is (160-2Rolling the vulcanized and cut rubber floor for at least 12 hours with the effective vulcanization time of (4-20) + -0.1 min and the cut width of 1218 +/-1 mm;
v. polishing
And D, polishing the back of the rubber floor by using the film after the step IV is parked on a polishing machine, and then, blanking in the length direction according to the requirement of the length of the rubber floor to obtain a rubber floor product.
Table 2 shows the results of the hydrophobicity and mechanical property tests of the rubber flooring products prepared from the rubber raw material compositions of comparative examples 1 to 5.
TABLE 2
By comparing the performance test results of the samples in table 2, it can be seen that:
1. the rubber floor made of the silicon rubber as the main material has good hydrophobic property, but has low mechanical property, and cannot reach the related product standard of the elastic rubber floor.
2. The rubber floor made of the EPDM rubber as the main material has poor surface hydrophobicity and poor surface cleaning effect, and cannot achieve the self-cleaning effect.
3. The rubber floor prepared by singly taking the EVA resin as the main material has low hydrophobicity, high hardness, low elongation at break and poor elasticity.
4. As can be seen from comparative example 4, the EPDM and silica gel were mixed in a ratio of 1: 1 as a main material, the prepared rubber floor has certain hydrophobic characteristics on the surface, but is influenced by higher content of silica gel, and the physical and mechanical properties (tear strength and tensile strength) of the product are lower.
5. From comparison of comparative examples 4 and 5, it is found that when the content of other materials in the composition is kept constant, EPDM, EVA resin and silica gel are mixed according to a certain proportion as main materials, and the content ratio of silica gel in the composition is reduced while a small amount of EVA resin is added, the mechanical properties of the rubber flooring product can be remarkably improved, and at the same time, the good surface hydrophobic property can be kept.
Experimental group 2
Comparative examples 6 to 10 provide rubber flooring material compositions having different relative amounts of the host material. The difference between the respective proportions is the amount of the added body material, and Table 3 shows the compositions in parts by weight of the rubber floor material compositions of comparative examples 6 to 10.
TABLE 3
Preparing the rubber floor raw material composition in each proportion into a rubber floor (specifically, a floor block or floor cloth) according to the following method:
I. first stage internal mixing
The ethylene propylene diene monomer, the EVA resin and the silicon rubber with the weight are put into an internal mixer, the internal mixing temperature is 60-90 ℃, the internal mixing pressure is 20-40kg, the rotor speed is 30-50r/min, and the internal mixing is carried out for 60-80 s; then adding modified aluminum hydroxide, modified white carbon black, nano zinc oxide, stearic acid and polyethylene glycol in sequence, wherein the banburying temperature is 90-160 ℃, the banburying pressure is 45kg, the rotor rotation speed is 40-50r/min, the banburying is 90-150s, the banburying and rubber discharging temperature is 150-;
II, second-stage banburying
Putting the materials subjected to banburying in the step I into a banbury mixer according to parts by weight, adding a vulcanizing agent, banburying at 70-110 ℃, banburying pressure within (20-50) kg, rotor rotating speed within (15-50) r/min, banburying for 90-150s, banburying rubber-removing temperature within 100-120 ℃, sheet-discharging, cooling and standing for at least more than 8 hours;
extrusion calendering III
Extruding the material in the step II to form a rubber sheet by a cold-feeding wide extruder, wherein the temperature of a machine head of the extruder is (55-95) DEG C, and the temperature of a machine body is as follows: (45-95) DEG C, the rotating speed of a screw of the extruder is 5-15r/min, the temperature of a calendering roller is (45-80) DEG C, and the rubber sheet is parked for at least 4 hours;
IV, vulcanizing and cutting edges
Vulcanizing and molding the film extruded in the step III on a drum vulcanizer, and simultaneously performing online trimming of two-side flash, wherein the control range of the vulcanization temperature is (160-2Rolling the vulcanized and cut rubber floor for at least 12 hours with the effective vulcanization time of (4-20) + -0.1 min and the cut width of 1218 +/-1 mm;
v. polishing
And D, polishing the back of the rubber floor by using the film after the step IV is parked on a polishing machine, and then, blanking in the length direction according to the requirement of the length of the rubber floor to obtain a rubber floor product.
Table 4 shows the results of the hydrophobicity and mechanical property tests of the rubber flooring products prepared from the rubber raw material compositions of comparative examples 6 to 10.
TABLE 4
By comparing the performance test results of the samples in table 4, it can be seen that:
1. the total weight part sum of the three main materials is kept to be 100, and when the proportion of the silica gel in the main materials is more than 30%, the rubber floor prepared by the raw material composition has poor mechanical property and can not meet the requirements of the rubber floor product standard (the tensile strength of the rubber floor is more than or equal to 8MPa, the elongation is more than or equal to 50%, and the tear strength is more than or equal to 30 KN/m).
2. When the weight ratio of the EPDM rubber in the main material is more than 60%, the tearing strength of the prepared rubber floor is higher and can reach more than 30.
3. When the weight ratio of the EVA resin in the main material reaches more than 30%, the hardness of the prepared rubber floor is higher; when the weight percentage of the EVA resin in the main material is 15-20%, the overall performance and the water contact angle of the rubber floor are not obviously different.
Experimental group 3
Comparative examples 11 to 15 provide rubber flooring raw material compositions containing different compositions of protective materials. Table 5 shows the compositions in parts by weight of the rubber floor material compositions of comparative examples 11 to 15.
TABLE 5
Preparing the rubber floor raw material composition in each proportion into a rubber floor (specifically, a floor block or floor cloth) according to the following method:
I. first stage internal mixing
The ethylene propylene diene monomer, the EVA resin and the silicon rubber with the weight are put into an internal mixer, the internal mixing temperature is 60-90 ℃, the internal mixing pressure is 40kg, the rotor speed is 30-50r/min, and the internal mixing is carried out for 60-80 s; then adding modified aluminum hydroxide, modified white carbon black, nano zinc oxide, stearic acid, oxidized polyethylene wax, erucamide and polyethylene glycol in sequence, wherein the banburying temperature is 90-160 ℃, the banburying pressure is 20-45kg, the rotor rotation speed is 40-50r/min, the banburying is 90-150s, the banburying and rubber-removing temperature is 150-;
II, second-stage banburying
Putting the materials subjected to banburying in the step I into a banbury mixer according to parts by weight, adding a vulcanizing agent, carrying out banburying at 70-110 ℃, controlling the banburying pressure range to be 20-50kg, controlling the rotor speed range to be 15-50r/min, carrying out banburying for 90-150s, controlling the banburying rubber discharge temperature to be 100-120 ℃, and carrying out sheet discharging, cooling and standing for at least more than 8 hours;
extrusion calendering III
Extruding the material in the step II into a rubber sheet by a cold-feeding wide extruder, wherein the temperature of a machine head of the extruder is 55-95 ℃, and the temperature of a machine body is as follows: the temperature is 45-85 ℃, the rotating speed of a screw of the extruder is 5-15r/min, the temperature of a calendering roller is 45-80 ℃, and the rubber sheet is parked for at least 4 hours;
IV, vulcanizing and cutting edges
Vulcanizing and molding the film extruded in the step III on a drum vulcanizer, and simultaneously performing online trimming of two-side flash, wherein the control range of the vulcanization temperature is (160-2Rolling the vulcanized and cut rubber floor for at least 12 hours with the effective vulcanization time of (4-20) + -0.1 min and the cut width of 1218 +/-1 mm;
v. polishing
And D, polishing the back of the rubber floor by using the film after the step IV is parked on a polishing machine, and then, blanking in the length direction according to the requirement of the length of the rubber floor to obtain a rubber floor product.
Table 6 shows the results of the hydrophobicity, mechanical properties and stability tests of the rubber flooring products prepared from the rubber raw material compositions of comparative examples 11 to 15.
TABLE 6
Table 6 (the same as table 8 below) tests for surface deposition were conducted to observe the surface deposition of the material at different times. The surface deposition is a phenomenon in which the material composition is brought into contact with air after molding, and a part of the compounding agent migrates from the inside of the rubber to the surface of the rubber with changes in the environment (temperature, humidity, ultraviolet rays, and hot air) and time. If the surface has a bleed-out, it is an indication that one or more materials in the composition are out of solubility in the rubber. The surface precipitation state is "normal", which means that the material surface is free from precipitation.
By comparing the performance test results of the samples in table 6, it can be seen that:
1. when the increase of the content of the oxidized polyethylene wax is beneficial to improving the hardness of the rubber floor product, the content of the oxidized polyethylene wax in the raw material composition is controlled to be 1-5 percent.
2. When the total weight of the polyethylene wax and the erucamide exceeds 2 percent of the total weight of the raw material composition, the product can be separated out to different degrees, and the total content of the oxidized polyethylene wax and the erucamide in the raw material is controlled to be 0.5 to 2 percent.
Experimental group 4
Examples 1 to 2 and comparative examples 16 to 22 provide rubber flooring material compositions, respectively. Table 7 shows the compositions of the respective rubber floor material compositions in parts by weight.
TABLE 7
The rubber floor raw material compositions of the above examples and comparative examples were prepared into rubber floors (specifically, floor boards or floor cloths) according to the following methods:
I. first stage internal mixing
The ethylene propylene diene monomer, the EVA resin and the silicon rubber with the weight are put into an internal mixer, the internal mixing temperature is 60-90 ℃, the internal mixing pressure is 40kg, the rotor speed is 30-50r/min, and the internal mixing is carried out for 60-80 s; then adding modified aluminum hydroxide, modified white carbon black, nano zinc oxide, stearic acid, oxidized polyethylene wax, erucamide and polyethylene glycol in sequence, wherein the banburying temperature is 90-160 ℃, the banburying pressure is 20-45kg, the rotor rotation speed is 40-50r/min, the banburying is 90-150s, the banburying and rubber-removing temperature is 150-;
II, second-stage banburying
Putting the materials subjected to banburying in the step I into a banbury mixer according to parts by weight, adding a vulcanizing agent, carrying out banburying at 70-110 ℃, controlling the banburying pressure range to be 20-50kg, controlling the rotor speed range to be 15-50r/min, carrying out banburying for 90-150s, controlling the banburying rubber discharge temperature to be 100-120 ℃, and carrying out sheet discharging, cooling and standing for at least more than 8 hours;
extrusion calendering III
Extruding the material in the step II to form a rubber sheet by a cold-feeding wide extruder, wherein the temperature of a head of the extruder is 55-95 ℃, the temperature of a machine body is 45-85 ℃, the rotating speed of a screw rod of the extruder is 5-15r/min, the temperature of a calendering roller is 45-80 ℃, and the rubber sheet is kept for at least 4 hours;
IV, vulcanizing and cutting edges
Vulcanizing and molding the film extruded in the step III on a drum vulcanizer, and simultaneously performing online trimming of two-side flash, wherein the control range of the vulcanization temperature is (160-2Rolling the vulcanized and cut rubber floor for at least 12 hours with the effective vulcanization time of (4-20) + -0.1 min and the cut width of 1218 +/-1 mm;
v. polishing
And D, polishing the back of the rubber floor by using the film after the step IV is parked on a polishing machine, and then, blanking in the length direction according to the requirement of the length of the rubber floor to obtain a rubber floor product.
Table 8 shows the results of the hydrophobicity, mechanical properties and stability tests of the rubber flooring products prepared from the rubber raw material compositions according to the above examples and comparative examples.
TABLE 8
By comparing the performance test results of each rubber floor sample in table 8, it can be seen that:
1. the mechanical property and the fire-proof performance of the rubber floor provided by the embodiment can meet the basic requirements of industrial products. Further, the rubber floors of the embodiment 1 and the embodiment 2 meet the technical standards of floor cloth for Q/CR617-2017 passenger trains and motor train units, the GB/T8624-2012 building materials and products in combustion performance classification B1, the HGT3747.1-2011 rubber and plastic floor material part 1, and the HL3 safety level under EN 45545-2R 10.
2. In the rubber floor samples of comparative examples 16 to 22 in table 8, the oxygen index of the rubber floor of comparative example 16 and comparative example 17, the tear strength of the rubber floor of comparative example 18, the TVOC results of the rubber floor of comparative example 20 and comparative example 22, the grip grade of the rubber floor of comparative example 21 and comparative example 22 did not meet the relevant industrial standard requirements, and the surface bleeding of the rubber floor 4320h of comparative example 21 and comparative example 22 was a case where the relevant industrial standard was not potentially met.
The above results show that the selection of proper polyethylene wax and amide compound has different influences on the fire resistance, mechanical property, anti-skid property and temperature resistance of the rubber floor by adopting the hydrophobically modified aluminum hydroxide and the hydrophobically modified white carbon black and controlling the dosage of the hydrophobically modified aluminum hydroxide and the hydrophobically modified white carbon black.
In conclusion, the rubber floor prepared from the raw material composition can meet the basic requirements of the industry on the mechanical performance, low-smoke fireproof performance and halogen-free environment-friendly performance of the rubber floor by selecting proper raw material components and controlling the dosage of each component within a specific range, and a hydrophobic substrate hardened layer can be formed on the surface of the floor, so that the effects of isolating from stains and self-cleaning are achieved, waxing is not needed, and the rubber floor is suitable for various scenes for elastic floor decoration.
Claims (15)
1. A rubber floor raw material composition comprises the following components in parts by weight: 50-80 parts of ethylene propylene diene monomer, 5-25 parts of silicone rubber, 5-25 parts of EVA resin, 3-8 parts of zinc oxide, 0.5-3 parts of stearic acid, 1-7 parts of oxidized polyethylene wax, 0.4-2.2 parts of erucamide, 0.3-4 parts of polyethylene wax, 0.5-2.5 parts of polyethylene glycol, 100-200 parts of hydrophobic group modified aluminum hydroxide, 15-40 parts of hydrophobic group modified white carbon black and 1.5-6 parts of vulcanizing agent.
2. The rubber flooring raw material composition according to claim 1, wherein the ethylene propylene diene monomer, the silicone rubber and the EVA resin are used as a main material, the weight ratio of the silicone rubber in the main material is 18 to 36%, the weight ratio of the ethylene propylene diene monomer in the main material is 40 to 80%, and the weight ratio of the EVA resin in the main material is 12 to 30%, preferably 15 to 20%; preferably, the weight percentage of the main material in the rubber floor raw material composition is 24-55%.
3. The rubber flooring material composition of claim 1 or 2, wherein the ethylene propylene diene monomer rubber comprises a Dow chemical EPDM4570 type ethylene propylene diene monomer rubber.
4. The rubber flooring material composition of any one of claims 1-3, wherein the silicone rubber comprises a methyl vinyl silicone rubber.
5. The rubber flooring material composition of any one of claims 1 to 4, wherein the EVA resin comprises EVA 18.
6. The rubber flooring stock composition of claim 1, wherein the polyethylene wax comprises 1-5% of the total weight of the rubber flooring stock composition;
preferably, the sum of the weight of the polyethylene wax and the weight of the erucamide accounts for 0.5 to 2 percent of the total weight of the rubber floor raw material composition.
7. The rubber flooring stock composition of claim 1, wherein the oxidized polyethylene wax comprises OPE 90;
the polyethylene wax includes polyethylene wax 1040P.
8. The rubber flooring raw material composition of claim 1, wherein the erucamide comprises erucamide having an erucic acid content of 90% in the raw material.
9. The rubber flooring material composition of claim 1, wherein the vulcanizing agent includes a peroxide vulcanizing agent and/or a vulcanization aid.
10. The rubber flooring material composition of claim 1, wherein the polyethylene glycol comprises polyethylene glycol 6000.
11. The rubber flooring material composition of claim 1, wherein the zinc oxide comprises nano zinc oxide, preferably the nano zinc oxide has a particle size of 10-100 μ ι η.
12. A rubber floor produced from the rubber floor material composition as recited in any one of claims 1 to 11.
13. The method for producing a rubber floor as claimed in claim 12, comprising: and sequentially carrying out first-stage banburying, second-stage banburying, extrusion calendering, vulcanization edge cutting and polishing on the rubber floor raw material composition to obtain the rubber floor.
14. The preparation method according to claim 13, wherein the temperature of the first-stage banburying rubber discharge is above 140 ℃, preferably above 150 ℃;
in the step of vulcanizing the cut edge, the vulcanizing temperature is (150-.
15. Use of the rubber floor of claim 12 in vehicles and architectural trim, preferably said vehicles comprise rail vehicles, ground buses, ships; more preferably, the rail transit vehicle comprises a railway high-speed passenger train, a common railway passenger train, a light rail vehicle, a tramcar, a subway vehicle, an urban rail and a magnetic levitation vehicle.
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