CN113717475B - 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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- CN113717475B CN113717475B CN202111062507.6A CN202111062507A CN113717475B CN 113717475 B CN113717475 B CN 113717475B CN 202111062507 A CN202111062507 A CN 202111062507A CN 113717475 B CN113717475 B CN 113717475B
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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
-
- 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
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
- C08K2003/2227—Oxides; Hydroxides of metals of aluminium
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
- C08K2003/2296—Oxides; Hydroxides of metals of zinc
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/011—Nanostructured additives
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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
- C08L2201/00—Properties
- C08L2201/02—Flame or fire retardant/resistant
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02T—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO TRANSPORTATION
- Y02T30/00—Transportation of goods or passengers via railways, e.g. energy recovery or reducing air resistance
Abstract
The invention provides a rubber floor raw material composition, a rubber floor, a preparation method and application thereof. The rubber floor raw material composition comprises the following components: 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, and the preparation method comprises the steps of carrying out first-stage banburying, second-stage banburying, extrusion calendaring, vulcanization edge cutting and polishing on the rubber floor raw material composition in sequence to obtain the rubber floor. The invention further provides application of the rubber floor in vehicles and building decoration. The rubber floor has high hydrophobicity and good self-cleaning capability, does not need waxing in the use process, and has low maintenance cost.
Description
Technical Field
The invention relates to the technical field of building decoration materials, in particular to a self-cleaning and easy-cleaning rubber floor raw material composition, a rubber floor, a preparation method and application thereof.
Background
The rubber floor is an elastic flooring material with wide application, 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 has high elasticity polymer material with reversible deformation, and has strong elasticity at room temperature, and because the surface structure of the rubber is loose and the compactness is not strong, the surface of the rubber is relatively easy to be corroded by stains, thereby forming dirt, and the surface of the rubber is not easy to clean. In particular, the rubber floors on the market currently have the following problems:
1. at present, the rubber floor mainly depends on surface waxing to form a hardening isolation layer on the surface of the rubber floor cloth so as to solve the problem of poor stain resistance on the surface of the rubber floor, but the surface waxing of the rubber floor has a certain effect only in a short period of time;
2. the scratch resistance of the surface of the rubber floor is reduced after waxing, white marks can be left after the surface is scratched by a relatively hard object, and the decorative attractiveness of the rubber floor is seriously affected;
3. the surface waxing of the rubber floor or the household wood floor requires professional personnel to perform operation, so that the difficulty of daily maintenance is increased, and the maintenance cost of the whole life cycle of the product is also increased.
According to the standard requirements of rubber floors (cloths) in different industries, the related technical standards are mainly as follows:
conventional physical and mechanical properties: in order to ensure that the product has normal use capability in life cycle;
fireproof performance: the fire protection device meets the fire protection requirements of different industries, prevents the occurrence of harmful substances during combustion, prevents flame from spreading and generates thick smoke when the fire accident happens, and further prolongs the time and probability of escape and rescue.
The rubber floor (cloth) is one of the very important characteristics as the floor decorating material, the attractive performance of the product has very important effect on the product application besides the conventional physical and mechanical properties, the fireproof performance and the environmental protection performance, and the pollution resistance (easy cleaning) of the product is mainly measured by different solvent/solution resistance in different industry standards of the conventional rubber floor (cloth), so that the practical treading experiment and other experimental standards of the product are relatively few.
Similar hydrophobic self-cleaning use techniques and related technical patents and literature are not currently being searched for in the rubber flooring (cloth) or resilient flooring industry products.
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 waxing in the use process, and has low maintenance cost.
In order to achieve the aim, the invention provides a rubber floor raw material composition, which comprises, by weight, 50-80 parts of ethylene propylene diene monomer rubber, 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.
According to the invention, the silicone rubber, the ethylene propylene diene monomer and the EVA resin are added as main materials, and the polyethylene wax, the oxidized polyethylene wax and the erucic acid amide are used as high molecular protection materials and hydrophobic base materials to form the raw material composition of the rubber floor, so that the prepared rubber floor can meet the requirements of mechanical property, low smoke fireproof performance and halogen-free environmental protection performance of industry standard floor, and can obtain the floor surface with a hydrophobic hardening layer, thereby achieving the effects of isolation from stains and self cleaning. In some embodiments, the rubber flooring may be a rubber flooring block or a rubber flooring 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 host material, the weight ratio of the silicone rubber in the host material is 18-36% (e.g., 20%, 25%, 30%, 35%, etc.), the weight ratio of the ethylene propylene diene monomer in the host material is 40-80% (e.g., 50%, 60%, 70%, etc.), and the weight ratio of the EVA in the host material is 12-30%, e.g., 15-20%. The weight ratio of the main body material in the rubber floor raw material composition is generally controlled to be 24-55%. In some embodiments, the total parts by weight of the host material may be controlled to 100 parts.
In a specific embodiment of the present invention, the ethylene propylene diene monomer may comprise a Dow chemical EPDM4570 type ethylene propylene diene monomer.
In particular embodiments of the present invention, the silicone rubber may comprise methyl vinyl silicone rubber.
In particular embodiments of the present invention, the EVA resin may comprise EVA18, i.e., a series of EVA18 products, such as EVA18-3, EVA18J3, and the like, produced by Yanshan petrochemical industry.
In a specific embodiment of the present invention, the polyethylene wax, oxidized polyethylene wax and erucamide are protective 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 roles of stain isolation and self cleaning. The polyethylene wax forms a minor outer layer surface for increasing the adhesive strength between the oxidized polyethylene wax and the host material while also increasing the surface hardness of the rubber floor. In a specific embodiment, the polyethylene wax may be selected from polyethylene wax 1040P. The polyethylene wax generally comprises 1 to 5% by weight of the total weight of the rubber floor raw material composition. The sum of the weight of the polyethylene wax and the weight of the erucamide generally accounts for 0.5 to 2 percent 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 specific embodiment of the present invention, the oxidized polyethylene wax comprises OPE90 and the like.
In a specific embodiment of the invention, the erucic acid amide comprises erucic acid amide with 90% of erucic acid content in raw materials, the purity of the finished product of the erucic acid amide is higher, and the erucic acid amide content can reach more than 98%.
In the 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 1.5 to 5 parts by weight, 1.5 to 4 parts by weight, etc. The vulcanizing agent may include a peroxide vulcanizing agent and/or a vulcanization aid.
In a specific embodiment of the present invention, the polyethylene glycol may include polyethylene glycol 6000 and the like.
In a specific embodiment of the present 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 (3) sequentially carrying out primary banburying, secondary banburying, extrusion calendaring, 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 step of the first-stage banburying, the temperature of the first-stage banburying is 60-160 ℃ (e.g., 60-130 ℃ and 90-160 ℃), the pressure of the first-stage banburying is 10-55kg (e.g., 10-45kg and 20-45 kg), the rotation speed of the rotor is 20-50r/min (e.g., 40-50 r/min), and the time of the first-stage banburying is 90s-150s. The first stage banburying glue discharge temperature is generally 140 ℃ or higher, for example 150 ℃ or higher, so that the oxidized polyethylene wax can be sufficiently melted. In the first-stage banburying process, oxidized polyethylene wax begins to melt at the temperature of 95-100 ℃, and at the moment, the polyethylene wax can play a role in lubricating the internal structure of rubber, so that the compatibility between the rubber and other raw materials is improved, and the rubber is well dispersed in the raw materials; when the temperature reaches 140-150 ℃, the oxidized polyethylene wax begins to melt and then forms a hardened wax film on the surface of the rubber matrix.
In some embodiments, the above-described preparation method may be a first stage banburying after mixing the pre-banged host material with the other raw material composition without banburying. The conditions of the preliminary banburying undergone by the host material are generally: the banburying temperature is 40-90 ℃ (60-90 ℃ for example), the banburying pressure is 15-50kg (20-40 kg for example), the rotating speed of the rotor is 30-50, and the banburying time is 60-80s.
In the above preparation method, preferably, in the step of the second-stage banburying, the temperature of the second-stage banburying is 70-110 ℃, the pressure of the second-stage banburying is 10-55kg (for example, 20-50 kg), the rotating speed of the rotor is 15-50r/min, the time of the second-stage banburying is 90s-150s, and the glue discharging temperature of the second-stage banburying is 70-120 ℃.
In the above production method, preferably, in the step of extrusion calendering, the extruder head temperature is 45 to 95 ℃ (e.g., 45 to 85 ℃, 55 to 95 ℃), the body temperature is 45 to 95 ℃ (e.g., 45 to 85 ℃), the extruder screw speed is 5 to 15r/min, and the calender roll temperature is 45 to 80 ℃.
In the above-mentioned production method, in the step of vulcanizing the cut edges, the vulcanization temperature is generally controlled to be (150-190) ±2 ℃, for example (160-190) ±2 ℃, so that the oxidized polyethylene wax is first precipitated to form the outermost layer of the floor board, and the polyethylene wax is then precipitated to form the secondary outer layer of the floor board. In view of economic efficiency, it is generally possible to choose a vulcanization temperature of 180 ℃. The vulcanization pressure is generally (3.0-5.5). + -. 0.3kg/cm 2 The effective vulcanization time is (4-20) +/-0.1 min, and the edge width is 1218+/-1 mm.
The invention further provides application of the rubber floor in vehicles. In particular, the vehicles include, but are not limited to, rail transit vehicles, ground buses, boats, etc. The rail transit vehicle may include, but is not limited to, a rail high speed passenger train motor train unit, a general rail train, a light rail vehicle, a tram, a subway vehicle, a city rail, a magnetic levitation vehicle, and the like.
The invention also provides application of the rubber floor in building decoration. In particular, the building includes, but is not limited to, libraries, museums, hospitals, airports, kindergarten, micro-machine rooms, gymnasiums, geriatric homes, sports venues, office buildings, industrial plants, and the like.
Compared with the existing rubber floor (cloth) technology, the self-cleaning rubber floor for the floor covering flooring material provided by the invention 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 improves the combustion safety of products.
2. According to the preparation method of the rubber floor, the prepared rubber floor has the self-cleaning and easy-cleaning functions by reasonably preparing the formula, so that the difficulty that the product is difficult to clean in the use process is solved, waxing is avoided in the use process of the floor, the maintenance cost of the whole life cycle of the product is reduced, and the attractive effect of keeping the colorful color in the use process of the product is improved.
Detailed Description
The technical solution of the present invention will be described in detail below for a clearer understanding of technical features, objects and advantageous effects of the present invention, but should not be construed as limiting the scope of the present invention.
The experimental methods in the following examples were all conventional methods, and the various raw materials used in the following examples were all commercially available materials with the exception of the modified materials. Wherein:
ethylene propylene diene monomer is Dow chemical EPDM4570;
the silicone rubber is methyl vinyl silicone rubber;
the EVA resin is EVA resin 18;
the vulcanizing agent is a peroxide vulcanizing agent, and the manufacturer is Amara 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 Guangzhou new thin metallurgical chemical industry Co., ltd;
the aluminum hydroxide is hydrophobic modified aluminum hydroxide (hereinafter referred to as modified aluminum hydroxide), and the manufacturer is a new material of Zibolan, inc.;
the zinc oxide is nano zinc oxide PZT-15 with the grain diameter of 10-100 mu m, and the manufacturer is Nanjing Baoket New Material Co., ltd;
stearic acid, polyethylene wax, polyethylene glycol 6000, erucamide, oleamide, oxidized polyethylene wax, OPE90, are routinely commercially available.
The test items referred to below are made 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 (Shore hardness) test method.
The strength is measured according to GB/T528 test method of the tensile stress and strain properties of vulcanized rubber or thermoplastic rubber.
Tear Strength reference GB/T529 test methods for determination of tear Strength of vulcanized rubber or thermoplastic rubber (trouser, right-angle and crescent shaped samples).
The elongation at break is referred to GB/T528 test method for determination of tensile stress and strain properties of vulcanized rubber or thermoplastic rubber.
The contact angle of water drops is referred to the measurement method of hydrophobic pollutant detection contact angle of GB/T24368 glass surface. Generally, a contact angle of < 90 ° is referred to as non-hydrophobic (hydrophilic), a contact angle of > 90 ° is referred to as hydrophobic, and a contact angle of > 150 ° is referred to as superhydrophobic.
Oxygen index reference GB/T2406.2 "plastics. Combustion behaviour was determined by oxygen index method: room temperature test method.
Smoke density reference GB/T8323.2 "plastic smoke generation part 2: testing method of testing smoke density by single-chamber method.
TVOC is described in ISO 12219-2, "Interior air of road vehicles-Part 2:Screening method for the determination of the emissions of volatile organic compounds from vehicle interior parts and materials-Bag method".
The anti-slip rating is based on DIN 51130 test method for anti-slip test of floor.
Solvent resistance is described in ISO 26987, resilient floor coverings-Determination of staining and resistance to chemicals, standard test methods.
The test method of the water-resistant pen, the coffee-resistant pen, the tea stain-resistant pen, the oil-resistant pen and the water-resistant pen are all visually inspected by personnel, and refer to HG/T3828-2006 indoor water-based wood paint.
Experiment group 1
Comparative examples 1 to 5 provide rubber floor raw material compositions having different kinds of main material. Table 1 is the composition of the rubber floor raw material compositions of comparative examples 1 to 5 in parts by weight.
TABLE 1
The rubber floor raw material compositions of the respective comparative examples were prepared into rubber floors (specifically, floor boards or floor cloths) according to the following methods:
I. first-stage banburying
Adding one or more than two of ethylene propylene diene monomer rubber, EVA resin and silicone rubber into an internal mixer, wherein the internal mixing temperature is 40-90 ℃, the internal mixing pressure is 15-50kg, the rotor rotating speed is 15-25r/min, and the internal mixing time is 60-80s; then sequentially adding modified white carbon black, nano zinc oxide, stearic acid and polyethylene glycol, banburying at 60-130 ℃, banburying pressure at 10-45kg, rotor rotating speed at 20-50r/min, banburying for 90-150s, banburying glue discharging at 150-160 ℃, discharging, cooling and standing for at least more than 4 hours;
II, second stage banburying
Putting the banburying materials in the step I into an internal mixer according to parts by weight, adding a vulcanizing agent, wherein the banburying temperature is 70-110 ℃, the banburying pressure is 10-50 kg, the rotor rotating speed is 15-50r/min, the banburying is 90-150s, the banburying glue discharging temperature is 70-120 ℃, and the cooling and standing of a discharged piece are at least more than 8 hours;
III extrusion calendaring
Extruding the materials in the step II into films through a cold feed broad-width extruder, wherein the temperature of the extruder head is (45-95) DEG C, and the temperature of the extruder body is: (45-85) DEG C, the screw speed of the extruder is 5-15r/min, the temperature of the calendaring roller is 35-80℃, and the film is parked for at least 4 hours;
IV, vulcanization cutting edge
Vulcanizing the film extruded in the step III on a drum vulcanizing machine to form, and simultaneously performing online trimming of burrs on two sides, wherein the vulcanizing temperature is controlled to be 160-190 ℃ plus or minus 2, and the vulcanizing pressure is 3.0-5.5 plus or minus 0.3kg/cm 2 The effective vulcanization time is (4-20) +/-0.1 min, and the edges are cutRolling the vulcanized and cut rubber floor with the width 1218+/-1 mm, cooling and standing for at least 12 hours;
v. polishing
And (3) polishing the back surface of the rubber floor on a polishing machine by using the film parked in the step (IV), and blanking in the length direction according to the length requirement of the rubber floor after polishing to obtain a rubber floor product.
Table 2 is the results of the hydrophobicity and mechanical property tests of the rubber flooring products prepared according to the rubber raw material compositions of comparative examples 1 to 5.
TABLE 2
By comparing the performance test results of the respective samples in table 2, it can be seen that:
1. the rubber floor made of the silicon rubber alone as the main material has better hydrophobic property, but has lower mechanical property and can not reach the related product standard of the elastic rubber floor.
2. The rubber floor made of the EPDM rubber alone is poor in surface hydrophobicity and poor in surface cleaning effect, and cannot achieve the self-cleaning effect.
3. The rubber floor made of EVA resin alone is not high in hydrophobicity, and is high in hardness, low in elongation at break and poor in elasticity.
4. As can be seen from comparative example 4, EPDM was mixed with silica gel according to 1:1, and the prepared rubber floor has certain hydrophobic property on the surface, but is influenced by higher silica gel content, 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, when the content of other materials in the composition is kept constant, EPDM, EVA resin and silica gel are mixed according to a certain ratio as main materials, the content ratio of silica gel in the composition is reduced while a small amount of EVA resin is added, and the mechanical properties of the manufactured rubber flooring product can be significantly improved while also maintaining good surface hydrophobicity.
Experiment group 2
Comparative examples 6 to 10 provide rubber floor raw material compositions having different relative amounts of the host materials. The difference between the comparative examples is the amount of the main material added, and Table 3 shows the compositions in parts by weight of the rubber floor raw material compositions of comparative examples 6 to 10.
TABLE 3 Table 3
The rubber floor raw material compositions of the respective comparative examples were prepared into rubber floors (specifically, floor boards or floor cloths) according to the following methods:
I. first-stage banburying
Putting the ethylene propylene diene monomer rubber, EVA resin and silicone rubber with the weight into an internal mixer, wherein the internal mixing temperature is 60-90 ℃, the internal mixing pressure is 20-40kg, the rotating speed of a rotor is 30-50r/min, and the internal mixing time is 60-80s; then adding modified aluminum hydroxide, modified white carbon black, nano zinc oxide, stearic acid and polyethylene glycol in turn, banburying at 90-160 ℃, banburying pressure 45kg, rotor rotating speed 40-50r/min, banburying for 90-150s, banburying glue discharging at 150-160 ℃, cooling and standing for at least more than 4 hours;
II, second stage banburying
Putting the banburying materials in the step I into an internal mixer according to parts by weight, adding a vulcanizing agent, wherein the banburying temperature is 70-110 ℃, the banburying pressure is 20-50kg, the rotor rotating speed is 15-50r/min, the banburying is 90-150s, the banburying glue discharging temperature is 100-120 ℃, and the cooling and standing of a discharged piece are at least more than 8 hours;
III extrusion calendaring
Extruding the materials in the step II into films through a cold feed broad-width extruder, wherein the temperature of the extruder head is (55-95) DEG C, and the temperature of the extruder body is as follows: (45-95) DEG C, the screw speed of the extruder is 5-15r/min, the temperature of the calendaring roller is (45-80) DEG C, and the film is parked for at least 4 hours;
IV, vulcanization cutting edge
Vulcanizing the film extruded in the step III on a drum vulcanizing machine to form, and simultaneously performing online trimming of burrs on two sides, wherein the vulcanizing temperature is controlled to be 160-190 ℃ plus or minus 2, and the vulcanizing pressure is 3.0-5.5 plus or minus 0.3kg/cm 2 The effective vulcanization time is (4-20) +/-0.1 min, the edge cutting width 1218+/-1 mm is used for rolling the vulcanized and edge-cut rubber floor, and cooling and standing for at least 12 hours;
v. polishing
And (3) polishing the back surface of the rubber floor on a polishing machine by using the film parked in the step (IV), and blanking in the length direction according to the length requirement of the rubber floor after polishing to obtain a rubber floor product.
Table 4 shows the results of the hydrophobicity and mechanical properties test of the rubber flooring products prepared according to the rubber raw material compositions of comparative examples 6 to 10.
TABLE 4 Table 4
By comparing the performance test results of the respective samples in table 4, it can be seen that:
1. when the total weight of the three main materials is 100, and the proportion of the silica gel in the main materials is more than 30%, the rubber floor prepared from the raw material composition has poor mechanical properties and cannot meet the requirements of rubber floor product standards (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 tearing strength is more than or equal to 30 KN/m).
2. When the weight ratio of the EPDM rubber to the main body material is more than 60%, the tearing strength of the manufactured rubber floor is higher and can reach more than 30.
3. When the weight ratio of the EVA resin in the main body material is more than 30%, the hardness of the manufactured rubber floor is higher; when the weight ratio of the EVA resin in the main body material is 15-20%, the overall performance and the water contact angle of the rubber floor are not obviously different.
Experiment group 3
Comparative examples 11 to 15 provide rubber floor raw material compositions containing protective materials of different compositions. Table 5 shows the compositions in parts by weight of the rubber floor raw material compositions of comparative examples 11 to 15.
TABLE 5
The rubber floor raw material compositions of the respective comparative examples were prepared into rubber floors (specifically, floor boards or floor cloths) according to the following methods:
I. first-stage banburying
Putting the ethylene propylene diene monomer rubber, EVA resin and silicone rubber with the weight into an internal mixer, wherein the internal mixing temperature is 60-90 ℃, the internal mixing pressure is 40kg, the rotating speed of a rotor is 30-50r/min, and the internal mixing is 60-80s; then sequentially adding modified aluminum hydroxide, modified white carbon black, nano zinc oxide, stearic acid, oxidized polyethylene wax, erucamide and polyethylene glycol, wherein the banburying temperature is 90-160 ℃, the banburying pressure is 20-45kg, the rotor rotating speed is 40-50r/min, the banburying is 90-150s, the banburying glue discharging temperature is 150-165 ℃, and the cooling and standing of the discharged sheets are at least more than 4 hours;
II, second stage banburying
Putting the banburying materials in the step I into an internal mixer according to parts by weight, adding a vulcanizing agent, wherein the banburying temperature is 70-110 ℃, the banburying pressure is 20-50kg, the rotor rotating speed is 15-50r/min, the banburying is 90-150s, the banburying glue discharging temperature is 100-120 ℃, and cooling and standing a discharged sheet for at least more than 8 hours;
III extrusion calendaring
Extruding the materials in the step II into films through a cold feed broad-width 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 of the rolling roller is 45-85 ℃, the screw speed of the extruder is 5-15r/min, the temperature of the rolling roller is 45-80 ℃, and the film is parked for at least 4 hours;
IV, vulcanization cutting edge
Vulcanizing the film extruded in the step III on a drum vulcanizing machine to form, and simultaneously performing online trimming of burrs on two sides, wherein the vulcanizing temperature is controlled to be 160-190 ℃ plus or minus 2, and the vulcanizing pressure is 3.0-5.5 plus or minus 0.3kg/cm 2 The effective vulcanization time is (4-20) +/-0.1 min, the edge cutting width 1218+/-1 mm is used for rolling the vulcanized and edge-cut rubber floor, and cooling and standing for at least 12 hours;
v. polishing
And (3) polishing the back surface of the rubber floor on a polishing machine by using the film parked in the step (IV), and blanking in the length direction according to the length requirement of the rubber floor after polishing to obtain a rubber floor product.
Table 6 shows the results of the hydrophobicity, mechanical properties, and stability test of the rubber flooring products prepared according to the rubber raw material compositions of comparative examples 11 to 15.
TABLE 6
Table 6 (table 8 below, same) the test for surface precipitation was to observe the surface precipitation of the material over different times. Wherein, the surface precipitation is a phenomenon that after the material composition is molded, the material composition is contacted with air, and part of the compounding agent migrates from the inside of the rubber to the surface of the rubber along with the change of environment (temperature and humidity, ultraviolet rays and hot air) and time. If the surface has a precipitate, this indicates that one or more materials in the composition have exceeded their solubility in rubber. A surface precipitation state of "normal" indicates that there is no precipitation on the surface of the material.
By comparing the performance test results of each sample in table 6, it can be seen that:
1. when the increase of the content of the oxidized polyethylene wax is advantageous for increasing the hardness of the rubber floor product, it is preferable to control the content of the oxidized polyethylene wax in the raw material composition to 1 to 5%.
2. When the total weight of the polyethylene wax and the erucamide exceeds 2% of the total weight of the raw material composition, the product can be precipitated to different degrees, and the total content of the oxidized polyethylene wax and the erucamide in the raw material is controlled to be 0.5-2% more suitably.
Experiment group 4
Examples 1 to 2 and comparative examples 16 to 22 provide rubber floor raw material compositions, respectively. Table 7 shows the compositions of the respective rubber floor raw 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 banburying
Putting the ethylene propylene diene monomer rubber, EVA resin and silicone rubber with the weight into an internal mixer, wherein the internal mixing temperature is 60-90 ℃, the internal mixing pressure is 40kg, the rotating speed of a rotor is 30-50r/min, and the internal mixing is 60-80s; then sequentially adding modified aluminum hydroxide, modified white carbon black, nano zinc oxide, stearic acid, oxidized polyethylene wax, erucamide and polyethylene glycol, wherein the banburying temperature is 90-160 ℃, the banburying pressure is 20-45kg, the rotor rotating speed is 40-50r/min, the banburying is 90-150s, the banburying glue discharging temperature is 150-165 ℃, and the cooling and standing of the discharged sheets are at least more than 4 hours;
II, second stage banburying
Putting the banburying materials in the step I into an internal mixer according to parts by weight, adding a vulcanizing agent, wherein the banburying temperature is 70-110 ℃, the banburying pressure is 20-50kg, the rotor rotating speed is 15-50r/min, the banburying is 90-150s, the banburying glue discharging temperature is 100-120 ℃, and cooling and standing a discharged sheet for at least more than 8 hours;
III extrusion calendaring
Extruding the material in the step II into a film by a cold feed wide-width extruder, wherein the temperature of a machine 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 calendaring roller is 45-80 ℃, and the film is parked for at least 4 hours;
IV, vulcanization cutting edge
Vulcanizing the film extruded in the step III on a drum vulcanizing machine to form, and simultaneously performing online trimming of burrs on two sides, wherein the vulcanizing temperature is controlled to be 160-190 ℃ plus or minus 2, and the vulcanizing pressure is 3.0-5.5 plus or minus 0.3kg/cm 2 The effective vulcanization time is (4-20) +/-0.1 min, the edge cutting width 1218+/-1 mm is used for rolling the vulcanized and edge-cut rubber floor, and cooling and standing for at least 12 hours;
v. polishing
And (3) polishing the back surface of the rubber floor on a polishing machine by using the film parked in the step (IV), and blanking in the length direction according to the length requirement of the rubber floor after polishing to obtain a rubber floor product.
Table 8 shows the results of the hydrophobicity, mechanical properties, and stability test of the rubber flooring products prepared according to the rubber raw material compositions of the above examples and comparative examples.
TABLE 8
From comparison of the performance test results of each of the rubber floor samples in table 8, it can be seen that:
1. the mechanical property and the fireproof property 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 Q/CR617-2017 floor cloths for railway buses and motor train units, meet the B1 grade of the combustion performance grades of GB/T8624-2012 building materials and products, meet the technical standards of the 1 st part rubber floor of the HGT3747.1-2011 rubber-plastic floor materials, and meet the HL3 safety grade under the EN 45545-2R 10 grade.
2. Among the rubber flooring samples of comparative examples 16 to 22 in table 8, the oxygen index of the rubber flooring of comparative example 16 and comparative example 17, the tear strength of the rubber flooring of comparative example 18, the TVOC results of the rubber flooring of comparative example 20 and comparative example 22, the slip resistance level of the rubber flooring of comparative example 21 and comparative example 22 did not meet the requirements of the related industry standard, and there were cases where the surface precipitation of the rubber flooring 4320h of comparative example 21 and comparative example 22 was potentially not met the related industry standard.
The results show that the proper polyethylene wax and the amide compound have different degrees of influence on the fireproof performance, the mechanical performance, the anti-skid performance and the 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 summary, the rubber floor prepared from the raw material composition obtained by selecting proper raw material components and controlling the dosage of each component within a specific range can meet the basic requirements of the industry on the mechanical property, the low smoke fireproof property and the halogen-free environment-friendly property of the rubber floor, and can form a hydrophobic base material hardening layer on the surface of the floor, thereby achieving the effects of isolating from stains and self-cleaning, avoiding waxing, and being suitable for various elastic floor decorative scenes.
Claims (19)
1. A rubber floor raw material composition, wherein the rubber floor raw material composition comprises, in parts by weight: 50-80 parts of ethylene propylene diene monomer rubber, 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 erucic acid amide, 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;
the ethylene propylene diene monomer, the silicone rubber and the EVA resin are used as main materials, the weight ratio of the silicone rubber in the main materials is 18-36%, the weight ratio of the ethylene propylene diene monomer in the main materials is 40-80%, and the weight ratio of the EVA resin in the main materials is 12-30%; the weight ratio of the main body material in the rubber floor raw material composition is 24-55%;
the polyethylene wax accounts for 1-5% of the total weight of the rubber floor raw material composition; the sum of the weight of the polyethylene wax and the weight of the erucamide accounts for 0.5-2% of the total weight of the rubber floor raw material composition; the oxidized polyethylene wax includes OPE90; the polyethylene wax includes polyethylene wax 1040P.
2. The rubber floor raw material composition according to claim 1, wherein the EVA resin accounts for 15 to 20% by weight of the host material.
3. The rubber floor raw material composition according to claim 1, wherein the ethylene propylene diene monomer rubber comprises a dow chemical EPDM4570 ethylene propylene diene monomer rubber.
4. A rubber floor raw material composition according to any one of claims 1 to 3, wherein the silicone rubber comprises methyl vinyl silicone rubber.
5. A rubber floor raw material composition according to any one of claims 1 to 3, wherein the EVA resin comprises EVA18.
6. The rubber floor raw material composition according to claim 4, wherein the EVA resin comprises EVA18.
7. The rubber floor raw material composition according to claim 1, wherein the erucamide comprises erucamide having an erucic acid content of 90% in raw material.
8. The rubber floor raw material composition according to claim 1, wherein the vulcanizing agent comprises a peroxide vulcanizing agent and/or a vulcanization aid.
9. The rubber floor raw material composition according to claim 1, wherein the polyethylene glycol comprises polyethylene glycol 6000.
10. The rubber floor raw material composition according to claim 1, wherein the zinc oxide comprises nano zinc oxide.
11. The rubber floor raw material composition according to claim 10, wherein the particle size of the nano zinc oxide is 10 μm to 100 μm.
12. A rubber floor board prepared from the rubber floor board raw material composition according to any one of claims 1 to 11.
13. The method for producing a rubber floor as defined in claim 12, comprising: and sequentially carrying out first-stage banburying, second-stage banburying, extrusion calendaring, vulcanization edge cutting and polishing on the rubber floor raw material composition to obtain the rubber floor.
14. The preparation method of claim 13, wherein the first-stage banburying glue discharging temperature is 140 ℃ or higher;
in the step of vulcanizing the cut edges, the vulcanizing temperature is 148-192 ℃.
15. The method according to claim 14, wherein the first-stage banburying glue discharging temperature is 150 ℃ or higher.
16. The method of claim 14, wherein in the step of vulcanizing the cut edge, the vulcanizing temperature is 158 ℃ to 192 ℃.
17. Use of the rubber flooring of claim 12 in vehicles and architectural trim.
18. The use of claim 17, wherein the vehicle comprises a rail transit vehicle, a ground bus, a marine vessel.
19. The use of claim 18, wherein the rail transit vehicle comprises a rail high speed passenger train, a common rail car, a light rail vehicle, a tram, a subway vehicle, a city rail, a magnetic levitation vehicle.
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| JP2700830B2 (en) * | 1989-12-27 | 1998-01-21 | 日本合成ゴム株式会社 | Rubber laminate |
| JP3652960B2 (en) * | 2000-06-26 | 2005-05-25 | トヨタ車体株式会社 | Non-halogen polymer laminate for automotive floor mats |
| CN100445328C (en) * | 2003-03-28 | 2008-12-24 | 陶氏环球技术公司 | Low gloss thermoformable flooring structure |
| JP2005187720A (en) * | 2003-12-26 | 2005-07-14 | Kaneka Corp | Composition for waterproof sheet and waterproof sheet |
| DE102006034646A1 (en) * | 2006-07-24 | 2008-01-31 | Carl Freudenberg Kg | Flooring |
| EP2046258A4 (en) * | 2006-08-04 | 2010-03-03 | Playtex Products Inc | Lubricious compositions and articles made therefrom |
| CN100436530C (en) * | 2007-03-15 | 2008-11-26 | 上海交通大学 | Prepn process of thermoplastic wood-plastic composite material based on polyethylene vinyl acetate |
| CN106280021B (en) * | 2016-08-09 | 2018-09-14 | 中国铁道科学研究院金属及化学研究所 | Rubber floor covering cloth and the application of a kind of rubber floor covering cloth composition and its preparation |
| CN106751013A (en) * | 2016-11-24 | 2017-05-31 | 连云港德翔新材料有限公司 | A kind of silicon rubber and ethylene propylene diene rubber and with Prefabricated runway coiled material and preparation method thereof |
| DE102016124555A1 (en) * | 2016-12-15 | 2018-06-21 | Nora Systems Gmbh | Flooring and process for its production |
| CN107641230B (en) * | 2017-08-18 | 2020-02-28 | 西北矿冶研究院 | Sterilization mould-proof rubber floor manufactured by using acidized modified white ash |
| CN110092987A (en) * | 2019-05-20 | 2019-08-06 | 潍坊亚星化学股份有限公司 | Train floor cloth advanced composite material (ACM) and preparation method thereof |
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