CN114990899A - TPU composite material and preparation method thereof - Google Patents
TPU composite material and preparation method thereof Download PDFInfo
- Publication number
- CN114990899A CN114990899A CN202210561754.9A CN202210561754A CN114990899A CN 114990899 A CN114990899 A CN 114990899A CN 202210561754 A CN202210561754 A CN 202210561754A CN 114990899 A CN114990899 A CN 114990899A
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- tpu
- flame
- retardant
- polyester fiber
- mass
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- D06N3/00—Artificial leather, oilcloth or other material obtained by covering fibrous webs with macromolecular material, e.g. resins, rubber or derivatives thereof
- D06N3/007—Artificial leather, oilcloth or other material obtained by covering fibrous webs with macromolecular material, e.g. resins, rubber or derivatives thereof characterised by mechanical or physical treatments
- D06N3/0077—Embossing; Pressing of the surface; Tumbling and crumbling; Cracking; Cooling; Heating, e.g. mirror finish
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M2101/00—Chemical constitution of the fibres, threads, yarns, fabrics or fibrous goods made from such materials, to be treated
- D06M2101/16—Synthetic fibres, other than mineral fibres
- D06M2101/30—Synthetic polymers consisting of macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
- D06M2101/32—Polyesters
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- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M2200/00—Functionality of the treatment composition and/or properties imparted to the textile material
- D06M2200/30—Flame or heat resistance, fire retardancy properties
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06N—WALL, FLOOR, OR LIKE COVERING MATERIALS, e.g. LINOLEUM, OILCLOTH, ARTIFICIAL LEATHER, ROOFING FELT, CONSISTING OF A FIBROUS WEB COATED WITH A LAYER OF MACROMOLECULAR MATERIAL; FLEXIBLE SHEET MATERIAL NOT OTHERWISE PROVIDED FOR
- D06N2209/00—Properties of the materials
- D06N2209/06—Properties of the materials having thermal properties
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- D06N—WALL, FLOOR, OR LIKE COVERING MATERIALS, e.g. LINOLEUM, OILCLOTH, ARTIFICIAL LEATHER, ROOFING FELT, CONSISTING OF A FIBROUS WEB COATED WITH A LAYER OF MACROMOLECULAR MATERIAL; FLEXIBLE SHEET MATERIAL NOT OTHERWISE PROVIDED FOR
- D06N2209/00—Properties of the materials
- D06N2209/06—Properties of the materials having thermal properties
- D06N2209/067—Flame resistant, fire resistant
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06N—WALL, FLOOR, OR LIKE COVERING MATERIALS, e.g. LINOLEUM, OILCLOTH, ARTIFICIAL LEATHER, ROOFING FELT, CONSISTING OF A FIBROUS WEB COATED WITH A LAYER OF MACROMOLECULAR MATERIAL; FLEXIBLE SHEET MATERIAL NOT OTHERWISE PROVIDED FOR
- D06N2209/00—Properties of the materials
- D06N2209/10—Properties of the materials having mechanical properties
- D06N2209/105—Resistant to abrasion, scratch
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- D06N2209/00—Properties of the materials
- D06N2209/14—Properties of the materials having chemical properties
- D06N2209/143—Inert, i.e. inert to chemical degradation, corrosion resistant
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- D06N—WALL, FLOOR, OR LIKE COVERING MATERIALS, e.g. LINOLEUM, OILCLOTH, ARTIFICIAL LEATHER, ROOFING FELT, CONSISTING OF A FIBROUS WEB COATED WITH A LAYER OF MACROMOLECULAR MATERIAL; FLEXIBLE SHEET MATERIAL NOT OTHERWISE PROVIDED FOR
- D06N2209/00—Properties of the materials
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- D06N2209/00—Properties of the materials
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- D06N2209/00—Properties of the materials
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- D06N2209/1685—Wear resistance
Abstract
The invention relates to a TPU composite material, which comprises polyester fiber cloth, a flame-retardant resin coating layer and flame-retardant TPU surface glue; the flame-retardant resin coating layer wraps the polyester fiber cloth, and the flame-retardant TPU surface glue is arranged on the surface of one side of the polyester fiber cloth and is combined with the flame-retardant resin coating layer outside the polyester fiber cloth. And the flame retardant in the flame-retardant resin coating layer and the flame-retardant TPU surface glue are halogen-free flame retardants. The TPU composite material disclosed by the invention avoids the addition of a plasticizer by utilizing the intrinsic flexibility of the TPU, and avoids the problems of pollution, harm to human health and the like caused by the addition of the plasticizer and a stabilizer in the traditional PVC coiled material product. Meanwhile, the invention further optimizes the production process of the composite material, not only can the production cost be reduced, but also the improved process is more suitable for producing products with larger width, and the prepared TPU composite material product has light weight, high wear-resistant grade, long service life, high peel strength resistance and excellent low-temperature resistance.
Description
Technical Field
The invention relates to the technical field of commercial materials, in particular to a TPU composite material and a preparation method thereof.
Background
At present, the coiled materials popular in the market all use PVC as main materials, a large amount of phenolic plasticizers and a small amount of fillers are added in the processing process, the problem of plasticizer precipitation often occurs in the daily use process, the aging of adhesives between the coiled materials and ground base layers is accelerated, and the problems of product bulging, degumming and the like are further caused. The plasticizer is an environmental hormone, although the toxicity of the plasticizer to a human body is not clear, the long-term contact can cause the reduction of the immunity and the fertility; especially, the potential harm to children in the development stage of endocrine system and reproductive system is larger. In order to improve the thermal decomposition of PVC products in the processing process, the prior art adopts a large amount of thermal stability to relieve the phenomenon, but stabilizers (especially lead salt stabilizers, organic tin stabilizers, rare earth stabilizers) and the like are main sources of heavy metals in the PVC products; soluble heavy metal can be slowly separated out in the using process, can enter the human body after contacting products containing the soluble heavy metal for a long time, is very slowly metabolized and deposited in the human body, and after a certain amount of soluble heavy metal is exceeded, heavy metal poisoning can occur, so that diseases such as headache, dizziness, insomnia, amnesia, nerve confusion, arthralgia, calculus, cancer and the like are caused, and the damage to cells, organs, skin, bones and nerves of a digestive system and a urinary system is particularly serious.
In daily life, coiled material floor (plastic flooring) is commonly used in places with large pedestrian volume, the market demand is very wide, the plastic flooring for traffic vehicles, the plastic flooring for buildings, the plastic flooring for indoor floors, the plastic flooring for outdoor floors, various gymnasiums, swimming pools, sports tracks and the like, and the surface wear resistance of the product is an important index for measuring the quality of the product. According to EN 13329, the abrasion resistance of the product surface is up to AC5 or above. The surface wear resistance of the product is mainly determined by the thickness of the wear-resistant layer and the material of the wear-resistant layer. The conventional coiled material floor is made of PVC (polyvinyl chloride) as a main material, and the thickness of a PVC wear-resistant layer is usually more than 0.55mm when the PVC wear-resistant layer reaches the AC5 wear-resistant grade, so that the overall thickness of the coiled material is large. In addition, in order to reduce the warping of the coiled material floor caused by heating in the development process of the PVC coiled material floor, the filling rate (the ratio of PVC resin powder to the filler) of the base material is low, so that the phenomena of expansion with heat and contraction with cold of the product are obvious, the low-temperature resistance of the PVC material is poor, the PVC material can be embrittled and cracked at the temperature of-10 ℃, and the use of places with harsh environmental conditions can be limited.
Disclosure of Invention
Technical problem to be solved
In view of the defects and shortcomings of the prior art, the invention provides the TPU composite material and the preparation method thereof, which avoid the problems of pollution and harm to human health caused by using plasticizers and stabilizers in the traditional PVC coiled material product and the production process, and further optimize the production process of the composite material to prepare the TPU composite material with light weight, high wear-resistant grade, long service life, high peel strength and excellent low-temperature resistance. The preparation method is particularly suitable for processing the composite material with large width or ultra-large width.
(II) technical scheme
In order to achieve the purpose, the invention adopts the main technical scheme that:
in a first aspect, the invention provides a TPU composite material, which comprises polyester fiber cloth, a water-based flame-retardant resin coating layer and a flame-retardant TPU surface adhesive; the water-based flame-retardant resin coating layer wraps the polyester fiber cloth, and the flame-retardant TPU surface glue is arranged on the surface of one side of the polyester fiber cloth and is combined with the water-based flame-retardant resin coating layer outside the polyester fiber cloth; the flame retardants in the water-based flame-retardant resin coating layer and the flame-retardant TPU surface glue are halogen-free flame retardants; and a UV hardening protective film is arranged on the surface of the flame-retardant TPU surface glue.
Preferably, the material of the water-based flame-retardant resin coating layer is a polyurethane-modified resin or a water-based polymer resin mixed with a polyurethane-modified resin. Preferably, the combination mode is impregnation, drying and hot-pressing compounding.
In a second aspect, the present invention provides a method of preparing a TPU composite, comprising the steps of:
s1, soaking the polyester fiber cloth in the water-based flame-retardant resin paste, taking out, drying and curing to obtain the polyester fiber base material coated with the water-based flame-retardant resin; the flame retardant in the water-based flame-retardant resin paste is a halogen-free flame retardant;
s2, scattering a layer of flame-retardant TPU powder on the surface of the polyester fiber substrate, heating to 150 ℃ and 250 ℃ to melt the flame-retardant TPU powder, and rolling to form flame-retardant TPU surface glue; the preparation method of the flame-retardant TPU powder comprises the following steps: mixing TPU granules, a halogen-free flame retardant, a light stabilizer and a processing aid, and carrying out melt stirring, extrusion, granulation and grinding to powder under the heating condition;
s3, coating a UV coating on the surface of the flame-retardant TPU surface glue, and forming a UV hardening protective film on the flame-retardant TPU surface glue.
According to a preferred embodiment of the present invention, in S1, the resin in the water-based flame retardant resin paste is a urethane-modified resin.
According to a preferred embodiment of the present invention, in S1, the method for preparing the water-based flame retardant resin paste comprises: uniformly mixing 100 parts by mass of water-based polymer resin, 10-50 parts by mass of halogen-free flame retardant, 0-5 parts by mass of mildew-proof antibacterial agent, 100 parts by mass of water and 500 parts by mass of filling aid, and 100-200 parts by mass of filling aid; wherein the water-based polymer resin is a water-soluble polyurethane modified resin or a mixture of a polyurethane resin and other water-soluble polymer resins.
Preferably, the water-soluble polymer resin is one or more of polyacrylic resin, epoxy resin, phenolic resin, polyurethane resin, vinyl acetate-ethylene copolymer, modified cellulose and modified rubber. The mildew-proof and anti-microbial agent can inhibit the growth of microorganisms. The mildew-proof antibacterial agent can be inorganic mildew-proof antibacterial agent or organic mildew-proof antibacterial agent, and the inorganic mildew-proof antibacterial agent can be metal ion antibacterial agent of silver, copper, zinc and the like and metal oxide (such as titanium dioxide, zinc oxide and the like). The organic mildew-proof antibacterial agent mainly comprises phenolic compounds (substituted aromatic hydrocarbons), element organic compounds, nitrogen-containing organic matters, halogen-containing organic matters, sulfur-containing organic matters and the like. The filling aid can reduce the resin consumption and improve the hardness of the polyester fiber cloth, and the filling aid can be calcium silicate or silica fume and the like.
According to the preferred embodiment of the present invention, in S1, the polyester fiber cloth is impregnated with the water-based flame-retardant resin paste in an amount of 1-10kg per square material, and then dried and cured in an oven at 250 ℃ under 150 ℃.
According to the preferred embodiment of the invention, in S2, the preparation method of the flame retardant TPU powder material comprises the following steps: uniformly mixing 100 parts by mass of TPU granules, 5-50 parts by mass of halogen-free flame retardant, 1-10 parts by mass of light stabilizer, 10-30 parts by mass of processing aid and 0-100 parts by mass of filler, melting and stirring at the high temperature of 150-250 ℃, extruding, granulating, and finally grinding to prepare 10-50 mesh powder.
Preferably, the halogen-free flame retardant is one or more of silane coupling agent coated and modified magnesium hydroxide, aluminum hydroxide, red phosphorus, expandable graphite and ammonium polyphosphate; the light stabilizer is a benzotriazole compound, such as 2- (2 ' -hydroxy-3 ', 5 ' -dicumylphenyl) benzotriazole; the processing aid comprises a lubricant and a release agent, wherein the lubricant is stearic acid and salts thereof (such as zinc stearate), and the release agent is one or more of silicone oil, silicone grease, silicone rubber and the like; the filler can be calcium silicate (preferably calcium silicate with good processability), silica aerogel, silica fume, calcium carbonate and the like. The filler can adjust the hardness and the wear resistance of the flame-retardant TPU surface glue, improve the heat resistance and the size stability of the product, save TPU granules and reduce the cost.
According to the preferred embodiment of the invention, in S2, flame retardant TPU powder is spread on the surface of the polyester fiber substrate through a powder spreading process, the thickness of the powder is controlled by the powder spreading amount, and the powder spreading amount is adjusted by the powder spreading speed and the powder spreading time; after the powder spreading is finished, the flame-retardant TPU powder is melted by heating through a high-temperature oven at the temperature of 150-250 ℃, and then the flame-retardant TPU surface adhesive is formed by rolling.
According to the preferred embodiment of the present invention, between S2-S3, the process steps of particulate scattering and surface cold pressing are also included; and embedding the particles scattered on the surface of the flame-retardant TPU surface adhesive into the TPU surface adhesive through a surface cold pressing process. Preferably, embossing is also formed on the surface of the flame retardant TPU surface glue through a surface cold pressing process. When the particles are TPU colorful particles, after the particles are embedded into the TPU surface glue, the particles are electrically heated at the temperature of 500 ℃ through 200 plus materials, the particles are melted, and the required texture is obtained on the TPU surface glue through cold embossing.
The scattered particles can be TPU colorful particles or carborundum particles or decorative particles or anti-slip/wear-resistant particles made of other materials scattered according to requirements. The TPU colorful particles mainly play a role in decoration, and the preparation method comprises the following steps: mixing 100 parts by mass of TPU granules, 5-50 parts by mass of halogen-free flame retardant and 1-10 parts by mass of colorant, and preparing into colored particles with different shapes and sizes by casting, cutting, crushing, sieving and other processes.
According to a preferred embodiment of the present invention, in S3, the UV paint is a functional UV paint; the coating mode is brush coating, spray coating or curtain coating, preferably brush coating, and the coating amount is 5-20g of the functional UV coating per square of the surface. The UV hardening protective film has the functions of scraping resistance, wear resistance, iodine tincture resistance, oil stain resistance, smoke prevention, scalding prevention and the like.
According to a preferred embodiment of the present invention, the preparation method further comprises step S4: after cooling, a back pressure process is adopted to press texture on the side opposite to the flame-retardant TPU surface glue, and the depth of the texture is preferably 0.10-0.30 mm. Therefore, the warping degree of the TPU composite material after being heated is reduced.
According to the preferred embodiment of the present invention, before S1 or between S1 and S2, a painting step is included: and (3) spraying and painting decorative patterns on the surface of the polyester fiber cloth or the surface of the polyester fiber base material on line. Preferably, the painting step is between steps S1 and S2.
In a third aspect, the present invention provides a TPU composite prepared by the method of any one of the above embodiments; the TPU composite material is a coiled material or a sheet or floor leather which takes TPU as surface glue.
(III) advantageous effects
The main technical effects of the invention comprise:
(1) the invention adopts thermoplastic polyurethane elastomer (TPU) and polyester fiber cloth as main materials to prepare the composite material which takes TPU as surface glue, and the technology carries out halogen-free flame retardant modification on TPU granules and a polyester fiber layer, so that the fire-proof grade of the composite material can be comparable to that of a PVC coiled material floor, and the composite material reaches B1 grade or even higher grade. Because the TPU material has better high wear resistance, the TPU surface glue with the thickness of 0.20mm can reach the wear resistance grade of the PVC surface glue floor leather with the thickness of 0.55 mm. The prepared TPU composite coiled material has light weight, and can effectively reduce the transportation cost, the load bearing of a carrier and the like. The TPU material has high elasticity, and has intrinsic flexibility, larger elongation at break and flexibility, so that no processing aids such as plasticizer and the like are added in the processing process, the problems of plasticizer precipitation and environmental pollution are avoided in the use process, and the problems of aging and separation of the adhesive between a product and the ground (an attachment surface) caused by plasticizer precipitation are avoided. The TPU material has excellent low temperature resistance and low temperature resilience, can still maintain the original elasticity and toughness at minus 30 ℃, and has the normal temperature and low temperature impact resistance far superior to that of PVC floor leather. Therefore, the composite material prepared by the invention and taking the TPU as the surface glue has wide application environment, and is particularly suitable for being used in some specific fields, such as environments with large bending amplitude and low temperature.
(2) In the process of preparing the TPU composite material, firstly, the water-based flame-retardant resin paste is used for carrying out impregnation treatment on the polyester fiber cloth, and the treatment process has at least the following excellent technical effects: firstly, by impregnating the polyester fiber cloth, the hardness and the strength of the polyester fiber cloth can be improved, and the sinking degree of the product after being pressed is reduced; secondly, the polyester fiber cloth is dip-dyed and coated by the resin paste modified by the water-based flame retardant, so that the polyester fiber cloth also has flame retardant property, and the flame retardant property and the safety of the TPU composite material are improved; and thirdly, the water-based flame-retardant resin paste is used for impregnating the polyester fiber cloth, so that the bonding strength between the TPU surface glue and the bottom polyester fiber cloth can be greatly improved, and the problems of layering, bulging and the like of the TPU composite material in the using process along with time, chemical erosion, expansion with heat, contraction with cold and the like are prevented. Meanwhile, the bonding strength between the polyester fiber cloth and an attachment surface (such as a ground) can be improved, so that the TPU composite material is not easy to separate. And fourthly, after the polyester fiber cloth is soaked in the water-based flame-retardant resin paste and dried, the fibers form a cementing relation, the strength of the polyester fiber cloth is greatly improved, so that the strength and the durability of the TPU composite material are improved, the requirement on the strength of the polyester fiber cloth is reduced, and woven fiber cloth, even non-woven cloth and the like with lower unit gram number can be used. In addition, when the woven rare polyester fiber cloth is used, complete patterns are difficult to spray on the surface of the polyester fiber cloth, but high-definition colorful patterns are easily formed on the surface of the polyester fiber cloth through water-based spraying after the polyester fiber cloth is pre-impregnated with water-based resin paste, dried, flattened and then sprayed.
(3) In the invention, the resin in the water-based flame-retardant resin paste is preferably polyurethane modified resin or mixed macromolecular resin containing polyurethane resin, so that the surface of the polyester fiber cloth impregnated with the water-based flame-retardant resin paste has resin molecular components (homogeneous materials are easy to combine into a whole) which are the same as those of the TPU surface glue, the combination firmness of the polyester fiber cloth and the TPU surface glue is further improved, and the stripping resistance is enhanced.
(4) The invention originally uses a powder spreading process when the TPU surface adhesive is formed, a layer of flame-retardant TPU powder is spread on the surface of the polyester fiber substrate, the flame-retardant TPU powder is melted by heating to 150-250 ℃, and the flame-retardant TPU surface adhesive is formed by rolling. The process has the main technical effects that the flame-retardant TPU powder is prepared by extruding, granulating and grinding TPU granules, a light stabilizer, a flame retardant and various auxiliaries, and all the components are fixed in the form of solid powder, so that the distribution of the components in the TPU powder is ensured to be very uniform, the stability of the adhesive surface performance of the TPU powder is improved, and the powder scattering process is more suitable for producing products with large width. Secondly, in the traditional technology, an extruder is used for extruding molten PVC and the like to a guide roller gap, and a guide roller rotates to carry out coating and calendaring molding, the length of the guide roller must be at least 30% greater than the width, so that the traditional calendaring technology is limited by equipment and is difficult to produce products with high width; in general, the prior art produces products of 1.0-2.0m width. The invention adopts the dusting process, can move the dusting device and the compression roller device (or a plurality of compression rollers) according to the width of the produced composite material so as to be convenient for producing high-width products, and is suitable for producing products with the width of 1.5-4.0m or more. The input cost of the traditional rolling equipment is high, and the input cost of the powder scattering device is low and is less than one fifth of that of the traditional rolling equipment. The powder scattering process has lower energy consumption and can effectively reduce the manufacturing cost of products. The traditional calendering or tape casting process has large processing limitation, and equipment needs to be continuously adjusted and modified due to different material properties; if high-hardness powder is doped in the material, the abrasion to equipment such as calendaring or tape casting is obvious, so that the equipment parameters need to be continuously adjusted adaptively, and high abrasion cost and high maintenance cost are brought. The traditional calendering or tape casting process has extremely high requirement on material fluidity, causes that the material viscosity cannot be too large, otherwise, the processing is difficult, and the process flexibility is limited. The invention adopts the powder scattering process, the TPU powder can be subjected to customized modification on the material components according to the market performance requirements, then the powder is ground into powder, and then the powder is scattered, the processability is strong, the process is simple to realize, the material components can be flexibly designed, and the production process cannot be influenced by the material performance.
(5) In the invention, the water-based flame-retardant resin paste and the flame-retardant TPU powder are both prepared by adopting the halogen-free flame retardant, the problem of using halogen elements and plasticizers in the traditional PVC coiled material is avoided, the environmental protection performance of the product is further upgraded, and the product can not volatilize toxic and irritant HCl gas during combustion. In some embodiments of the invention, the decorative effect can be achieved or the anti-slip and wear-resistant properties of the surface of the composite material can be enhanced by scattering particles such as TPU colorful particles or carborundum on the surface of the TPU surface adhesive and embedding the particles into the TPU surface adhesive by using a compression roller at normal temperature. In some embodiments of the invention, a UV hardening protective layer is formed on the surface of the TPU adhesive surface by methods such as film spraying and the like, so that the TPU adhesive surface has the functions of scraping resistance, wear resistance, iodine alcohol resistance, oil stain resistance, smoke prevention, scalding prevention and the like, and the service life of the material is prolonged.
Drawings
FIG. 1 is a flow chart of the method for preparing the TPU composite material according to the preferred embodiment of the invention.
Fig. 2 is a schematic structural diagram of the TPU composite material according to the preferred embodiment of the invention.
Detailed Description
For a better understanding of the present invention, reference will now be made in detail to the present embodiments of the invention, which are illustrated in the accompanying drawings.
The invention discloses a TPU composite material, which is a composite structure formed by taking polyurethane fiber cloth as a supporting material and TPU surface glue as a wear-resistant layer. In some embodiments, a UV hardening protective layer is formed on the surface of the TPU surface adhesive, so that the smoke-proof, scalding-resistant and cutting-resistant performances of the composite material are improved. The support material determines the specification and the size of the TPU composite material, such as the width, the unit weight and the structural stability of the product. The TPU surface adhesive mainly determines the wear resistance of the product.
As shown in fig. 1, the main production flow of the TPU composite material provided by the present invention is as follows: soaking water-based flame-retardant resin paste → drying → dusting → rolling, film forming → spreading particles → cold pressing and embossing → cooling → UV coating and laminating → cooling, back pressure shaping → trimming and rolling.
Among them, the implementation process of impregnating water-based type flame retardant resin paste and drying can be seen in the following method:
according to a set formula, 100 parts by mass of water-based polymer resin (preferably water-based polyurethane modified resin or mixture of water-based polyurethane resin and other water-based resin), 10-50 parts by mass of halogen-free flame retardant, 0-5 parts by mass of mildew-proof antibacterial agent, 100-500 parts by mass of water, 100 parts by mass of auxiliary filling agent and the like are sent to a stirring barrel through an automatic metering system, the materials in the stirring barrel are uniformly mixed by keeping the normal temperature at 25 +/-5 ℃ and stirring at 60 +/-5 RPM for 5-10min, and the viscosity of the mixed liquid is monitored to control the quality of the mixed liquid. Then, the polyester fiber layer with the width of 1.5-4.0m is soaked in the water-based polymer resin mixed solution through an unreeling process, and the soaking amount of each square material is controlled to be 1-10kg by adjusting the soaking time. Drying and curing the impregnated polyester fiber layer by an oven at the temperature of 150-250 ℃.
The implementation process of the steps of powdering and rolling to form the film can be seen in the following methods:
according to a set formula, 100 parts by mass of TPU granules, 5-50 parts by mass of halogen-free flame retardant, 1-10 parts by mass of anti-UV yellowing agent (light stabilizer), 10-30 parts by mass of processing aid, 0-100 parts by mass of filler (preferably calcium silicate with good processing performance) and the like are sent to a mixing barrel through an automatic metering system, melt stirring, extrusion, granulation and grinding are carried out at the high temperature of 150 plus one year at 250 ℃ to prepare 10-50-mesh powder, the ground powdery resin is uniformly spread on a polyester fiber layer through a powder spreading process, and the powder spreading amount is controlled through the powder spreading speed. And melting and bonding the spread TPU powder on the polyester fiber layer through a high-temperature oven at 250 ℃ under the condition of 150 plus materials, and then rolling to form a TPU surface adhesive layer, wherein the thickness of the TPU wear-resistant adhesive surface is 0.10-0.50 mm. Wherein, the thickness of the TPU surface layer is controlled by the dusting amount, and the dusting amount is adjusted by the dusting speed.
Wherein the steps of scattering, cold pressing and embossing are optional steps. In some embodiments, these three steps may not be present, in other embodiments only the spreading and cold pressing steps are present, or only the embossing step is present, in other embodiments three complete steps of spreading, cold pressing and embossing are present. The implementation of the three-step complete process can be seen in the following methods:
according to a set formula, 100 parts by mass of TPU granules, 5-50 parts by mass of halogen-free flame retardant, 1-10 parts by mass of processing aids such as colorant (usually 3-5 color master batches) and the like are mixed by automatic metering, and are processed into colorful particles with different shapes and sizes by tape casting, crushing, sieving and the like; then, the TPU colorful particles are scattered on the TPU surface adhesive layer, amorphous TPU colorful particles are embedded into the TPU surface adhesive layer through a cold pressing process, and then surface embossing treatment is carried out. The TPU colorful particles can be replaced by carborundum or other particle materials. The effect of the colorful particles is to enhance the decoration; the carborundum has the function of improving the wear resistance and skid resistance of the product.
Among them, UV coating lamination is a procedure in a preferred embodiment of the present invention. The UV coating lamination process can be seen in the following methods: a film spraying device is arranged on a polyester fiber cloth moving track, 5-20g of functional UV coating is coated on each square of the surface of the TPU adhesive surface through a film spraying process, and the coating is cured through an ultraviolet lamp to form a UV hardening protective film with the functions of scraping resistance, wear resistance, iodine tincture resistance, oil stain resistance, smoke prevention, scalding prevention and the like. Before UV film coating, the TPU rolled product can be cooled, and the surface temperature uniformity of the TPU rolled product is controlled.
The cooling and back pressure setting can be performed by the following methods: and cooling the product subjected to UV film coating treatment, pressing a 0.10-0.30mm deep bottom line on the surface of one side, opposite to the TPU glue surface, of the polyester fiber cloth through a backpressure shaping device, and reducing the heated warping degree of the TPU composite coiled material through cooling backpressure shaping. Finally, cutting the edge into 1.5-4.0m width or other preset widths, cooling and shaping (to reduce the normal temperature warping of the product), and winding at the center.
As shown in fig. 2, the TPU composite material according to the preferred embodiment of the present invention has a schematic structure. The bottom of the base material is a polyester fiber cloth base material A coated with water-based flame-retardant resin paste, a TPU surface glue layer B is combined above the polyester fiber cloth base material A, and a UV hardening protective film C is formed on the TPU surface glue layer B. And a plurality of colorful decorative particles or wear-resistant/anti-slip particles D are embedded in the TPU surface glue layer B.
The technical effects of the present invention will be further described below with reference to the properties of the products prepared by the specific examples. The formulation of the functional UV coating used in the following examples is as follows: 80kg of aqueous aliphatic polyurethane acrylate oligomer emulsion, 8kg of film forming additive, 2kg of photoinitiator, 1kg of flatting agent, 2kg of wetting agent, 1kg of defoaming agent, 3kg of glycerol, 10kg of reinforcing fiber and 8kg of deionized water. The reinforcing fiber is prepared from the following components in percentage by mass 2: 1 mixed wood and glass fibers.
Example 1
This example prepares a TPU composite by the following steps:
(1) 100 parts by mass of polyacrylic resin, 20 parts by mass of silane coupling agent coated and modified magnesium hydroxide, 2 parts by mass of organic mildew-proof antibacterial agent, 400 parts by mass of water, 100 parts by mass of calcium silicate and the like are conveyed into a stirring barrel through an automatic metering system, the stirring barrel is kept at the normal temperature of 30 ℃ and at the low speed of 65RPM for 10min, and all materials in the stirring barrel are uniformly mixed to obtain the halogen-free flame retardant modified water-based flame-retardant resin paste. Then, the polyester fiber cloth is soaked in the water-based flame-retardant resin paste through an unreeling process, and the soaking amount is 3 kg/square meter. And drying and curing the impregnated polyester fiber cloth by using a 200 ℃ oven to obtain the flame-retardant polyester fiber base material.
(2) 100 parts by mass of TPU granules, 25 parts by mass of silane coupling agent coated and modified magnesium hydroxide, 4 parts by mass of benzotriazole compound, 12 parts by mass of zinc stearate, 10 parts by mass of silicone oil, 15 parts by mass of calcium silicate and the like are fed into a mixing barrel through an automatic metering system, the materials are subjected to melt stirring, extrusion, granulation and grinding at a high temperature of 250 ℃ to prepare 20-30-mesh powder, the ground powder resin is uniformly spread on a polyester fiber substrate through a powder spreading process, and the powder spreading amount is controlled through the powder spreading speed. And (3) fusing the spread TPU powder on a polyester fiber base material through a high-temperature oven at 250 ℃, and then rolling to form a TPU wear-resistant glue surface, wherein the thickness of the wear-resistant glue surface is 0.20 mm.
(3) And (4) carrying out surface embossing treatment by adopting a cold pressing process. Then, by a UV film spraying process, about 15g of water-based iodine tincture-resistant UV coating is coated on each square of the surface, and is cured by an ultraviolet lamp to form a surface protection film with the functions of scraping resistance, wear resistance, iodine tincture resistance, oil stain resistance, smoke prevention, scalding prevention and the like. Finally, the product is pressed into shading with the depth of 0.15mm by cooling and back pressure processes, and then the product is cut to 2m width and rolled.
Example 2
The main difference between the present example and example 1 lies in the difference in the ingredients of the water-based flame-retardant resin paste, specifically, 100 parts by mass of the polyacrylic resin in step (1) is replaced by a mixed resin prepared by compounding aqueous polyurethane and polyacrylic resin in a mass ratio of 6: 4.
Example 3
The main difference between this example and example 1 is that the formulation of the aqueous flame-retardant resin paste is different, specifically, 100 parts by mass of the polyacrylic acid resin in step (1) is replaced with 100 parts of the aqueous polyurethane-modified resin.
Example 4
The embodiment prepares a TPU composite material with colorful particle decoration on the surface, and the preparation steps are as follows:
(1) 100 parts by mass of polyacrylic resin, 20 parts by mass of silane coupling agent coated and modified magnesium hydroxide, 2 parts by mass of organic mildew-proof antibacterial agent, 400 parts by mass of water, 100 parts by mass of calcium silicate and the like are conveyed into a stirring barrel through an automatic metering system, the stirring barrel is kept at the normal temperature of 30 ℃ and at the low speed of 65RPM for 10min, and all materials in the stirring barrel are uniformly mixed to obtain the halogen-free flame retardant modified water-based flame-retardant resin paste. Then, the polyester fiber cloth was impregnated in the water-based flame-retardant resin paste by an unreeling process, the impregnation amount being 3 kg/square meter. And drying and curing the impregnated polyester fiber cloth by using a 200 ℃ oven to obtain the flame-retardant polyester fiber base material.
(2) 100 parts by mass of TPU granules, 25 parts by mass of silane coupling agent coated and modified magnesium hydroxide, 4 parts by mass of benzotriazole compound, 12 parts by mass of zinc stearate, 10 parts by mass of silicone oil, 15 parts by mass of calcium carbonate and the like are fed into a mixing barrel through an automatic metering system, the materials are subjected to melt stirring, extrusion, granulation and grinding at a high temperature of 250 ℃ to prepare 20-30-mesh powder, the ground powder resin is uniformly spread on a polyester fiber substrate through a powder spreading process, and the powder spreading amount is controlled through the powder spreading speed. And (3) fusing the spread TPU powder on a polyester fiber base material through a high-temperature oven at 250 ℃, and then rolling to form the TPU wear-resistant adhesive surface. The thickness of the TPU wear-resistant rubber surface is 0.20 mm.
(3) And under the condition that the TPU wear-resistant rubber surface is not completely cooled and solidified, uniformly scattering TPU colorful particles on the TPU wear-resistant rubber surface. And embedding amorphous TPU colorful particles into the surface layer of the TPU through a cold pressing process, and then carrying out surface embossing treatment. The preparation method of the TPU colorful particles comprises the following steps: taking 9 parts by mass of 100 parts by mass of TPU granules, 20 parts by mass of silane coupling agent coated and modified magnesium hydroxide and three color concentrates, mixing the materials by automatic metering, casting to obtain a colorful sheet, and processing the colorful sheet into colorful particles with different shapes and sizes by a crusher and a vibrating screen.
(4) Through a UV film coating process, about 15g of functional UV coating is coated on each square of the surface, and the surface is cured through an ultraviolet lamp to form a layer of surface protection film with the functions of scraping resistance, wear resistance, iodine tincture resistance, oil stain resistance, smoke prevention, scalding prevention and the like. Finally, the product is pressed into shading with the depth of 0.15mm by cooling and back pressure processes, and then the product is cut to 2m width and rolled.
Example 5
The main difference between this example and example 4 lies in the different formulation of the water-based flame retardant resin paste, specifically, the TPU glittering particles scattered in step (3) are replaced by equal amount of carborundum, and the diamond is 36 meshes.
Example 6
The present example is mainly different from example 1 in that a polyester fiber cloth woven more sparsely and having more pores (lower weaving gram number) is used as a composite base material, and the impregnation amount of the water-based flame-retardant resin paste impregnated in step (1) is about 7.0 kg/m.
Comparative example 1
Commercial PVC flooring was purchased with a PVC thickness of 0.30 mm.
Comparative example 2
The present example is different from example 1 mainly in that the unreeled polyester fiber cloth is not impregnated with the water-based flame retardant resin paste, and flame retardant TPU powder of a certain thickness is directly spread thereon, and then the TPU composite material is produced according to the conditions and procedures of example 1.
The key indexes of the composite coils of the above examples 1 to 6 and comparative examples 1 to 2 were tested, and the test results are as follows:
the test method of the above properties is as follows:
(1) wear resistance rating: according to EN 13329 standard, a 100mm diameter circle is sampled, and an S42 grinding wheel is adopted to match with a No. 0 abrasive belt through a Table abrasion tester.
(2) Peel strength: ISO 24345 standard, sample 50X 150mm, pass the test of the microelectronic servo tensile machine under the normal temperature.
(3) Heat shrinkage ratio: according to the ISO 23999 standard, a sample with the specification of 250 x 250mm is taken, the normal temperature size 1 is tested, the normal temperature size 2 is recovered after the sample passes through an oven at the temperature of 80 ℃/6 hours, and the change rates of the size 1 and the size 2 are compared.
(4) High-temperature warping: according to the ISO 23999 standard, a sample with the specification of 250mm is taken, and after the sample is dried in an oven at the temperature of 80 ℃ for 6 hours, the normal temperature is recovered, and the maximum value of the four corner warpage of the sample is obtained.
(5) Flexibility: and according to the ISO24344 standard, a sample with the specification of 50 × 250mm is taken, and a cylinder with a preset diameter is wound at a certain ambient temperature to judge whether the appearance of the sample is cracked or broken.
(6) Coefficient of friction: EN 13893 standard, sample 500 × 1000mm specification, adopt the coefficient of dynamic friction tester, test out corresponding coefficient of friction.
The results of the performance comparison show that the bending performance (normal temperature and low temperature) of the composite material adopting TPU as surface adhesive is obviously superior to that of the PVC floor leather sold in the market (comparative example 1). Comparing examples 1-6 with comparative example 2, it can be seen that the TPU composite material prepared by impregnating the polyester fiber cloth with the water-based flame retardant resin paste in advance has better peel resistance, is more durable, has relatively low thermal shrinkage and high-temperature warping degree, and is not easy to have the problems of delamination, bulging and the like due to chemical erosion, thermal expansion, cold contraction and the like in the using process. In the aspect of wear resistance, when the thickness of the rubber surface of the TPU composite material is 0.2mm, the wear resistance grade of the TPU composite material is superior to that of PVC floor leather with the rubber surface thickness of 0.30mm, and the thickness of the PVC rubber surface of the PVC floor leather must reach 0.55mm to reach the same wear resistance strength of AC5 grade. Therefore, the preparation method can prepare the commercial composite coiled material with smaller thickness and lighter weight, and the preparation procedures of pre-dipping the water-based resin paste, scattering TPU powder, hot melting, flattening, cooling and the like are adopted, so that the preparation method is more suitable for processing the composite material with large width or super large width compared with the traditional casting process.
Finally, it should be noted that: the above embodiments are only used to illustrate the technical solution of the present invention, and not to limit the same; while the invention has been described in detail and with reference to the foregoing embodiments, it will be understood by those skilled in the art that: the technical solutions described in the foregoing embodiments may still be modified, or some or all of the technical features may be equivalently replaced; and the modifications or the substitutions do not make the essence of the corresponding technical solutions depart from the scope of the technical solutions of the embodiments of the present invention.
Claims (11)
1. The TPU composite material is characterized by comprising polyester fiber cloth, a water-based flame-retardant resin coating layer and flame-retardant TPU surface glue; the flame-retardant resin coating layer wraps the polyester fiber cloth, and the flame-retardant TPU surface glue is arranged on the surface of one side of the polyester fiber cloth and is combined with the flame-retardant resin coating layer outside the polyester fiber cloth; the flame retardant in the flame-retardant resin coating layer and the flame-retardant TPU surface glue are halogen-free flame retardants; and the surface of the flame-retardant TPU surface glue is also provided with a UV hardening protective film.
2. A preparation method of a TPU composite material is characterized by comprising the following steps:
s1, soaking the polyester fiber cloth in the water-based flame-retardant resin paste, taking out, drying and curing to obtain the polyester fiber base material coated with the water-based flame-retardant resin; the flame retardant in the water-based flame-retardant resin paste is a halogen-free flame retardant;
s2, scattering a layer of flame-retardant TPU powder on the surface of the polyester fiber substrate, heating to 150 ℃ and 250 ℃ to melt the flame-retardant TPU powder, and rolling to form flame-retardant TPU surface glue; the preparation method of the flame-retardant TPU powder comprises the following steps: mixing TPU granules, a halogen-free flame retardant, a light stabilizer and a processing aid, and carrying out melt stirring, extrusion, granulation and grinding to powder under the heating condition;
s3, coating a UV coating on the surface of the flame-retardant TPU surface glue, and forming a UV hardening protective film on the flame-retardant TPU surface glue.
3. The method according to claim 2, wherein in S1, the resin in the water-based flame-retardant resin paste is a polyurethane-modified resin.
4. The method according to claim 2, wherein in S1, the method for preparing the water-based flame-retardant resin paste comprises: uniformly mixing 100 parts by mass of water-based polymer resin, 10-50 parts by mass of halogen-free flame retardant, 0-5 parts by mass of mildew-proof antibacterial agent, 100 parts by mass of 500 parts by mass of water and 100-200 parts by mass of filling aid; wherein the water-based polymer resin is a water-soluble polyurethane modified resin or a mixture of the polyurethane modified resin and other water-soluble polymer resins.
5. The method of claim 2, wherein in S2, the flame retardant TPU powder is prepared by the following steps: uniformly mixing 100 parts by mass of TPU granules, 5-50 parts by mass of halogen-free flame retardant, 1-10 parts by mass of light stabilizer, 10-30 parts by mass of processing aid and 0-100 parts by mass of filler, melting and stirring at the high temperature of 150-250 ℃, extruding, granulating, and finally grinding to prepare 10-50 mesh powder.
6. The method according to claim 2, wherein in S2, flame retardant TPU powder is spread on the surface of the polyester fiber substrate by a dusting process, the powder thickness is controlled by the dusting amount, and the dusting amount is adjusted by the dusting speed and the dusting time; after the powder spreading is finished, the flame-retardant TPU powder is melted by heating through a high-temperature oven at the temperature of 150-250 ℃, and then the flame-retardant TPU surface adhesive is formed by rolling.
7. The method of claim 2, further comprising the steps of scattering the particles and cold surface pressing between S2 and S3; and embedding the particles scattered on the surface of the flame-retardant TPU surface adhesive into the TPU surface adhesive through a surface cold pressing process.
8. The preparation method of claim 7, wherein the particulate matter is TPU glittering particles, the TPU glittering particles are embedded in the TPU surface glue and then are heated at 200-500 ℃ to form a molten state, and the TPU surface glue is subjected to cold embossing treatment to obtain the required texture on the surface of the TPU surface glue.
9. The method according to claim 2, wherein in S3, the UV paint is a functional UV paint; the coating mode is brush coating, spray coating or curtain coating.
10. The method according to claim 2, further comprising step S4: after cooling, pressing texture on the side opposite to the flame-retardant TPU surface glue by adopting a back pressure process.
11. A TPU composite prepared by the process of any one of claims 2-10; the TPU composite material is a coiled material or a sheet or floor leather which takes TPU as surface glue.
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