CN115447244B - Sound-absorbing and sound-insulating multilayer film, composite structure thereof, wallpaper and preparation method - Google Patents
Sound-absorbing and sound-insulating multilayer film, composite structure thereof, wallpaper and preparation method Download PDFInfo
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- CN115447244B CN115447244B CN202211282899.1A CN202211282899A CN115447244B CN 115447244 B CN115447244 B CN 115447244B CN 202211282899 A CN202211282899 A CN 202211282899A CN 115447244 B CN115447244 B CN 115447244B
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- sound
- film
- layer
- absorbing
- composite structure
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Classifications
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- C08J9/06—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof using blowing gases generated by a previously added blowing agent by a chemical blowing agent
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
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- C09J163/00—Adhesives based on epoxy resins; Adhesives based on derivatives of epoxy resins
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- E—FIXED CONSTRUCTIONS
- E04—BUILDING
- E04B—GENERAL BUILDING CONSTRUCTIONS; WALLS, e.g. PARTITIONS; ROOFS; FLOORS; CEILINGS; INSULATION OR OTHER PROTECTION OF BUILDINGS
- E04B1/00—Constructions in general; Structures which are not restricted either to walls, e.g. partitions, or floors or ceilings or roofs
- E04B1/62—Insulation or other protection; Elements or use of specified material therefor
- E04B1/74—Heat, sound or noise insulation, absorption, or reflection; Other building methods affording favourable thermal or acoustical conditions, e.g. accumulating of heat within walls
- E04B1/82—Heat, sound or noise insulation, absorption, or reflection; Other building methods affording favourable thermal or acoustical conditions, e.g. accumulating of heat within walls specifically with respect to sound only
- E04B1/84—Sound-absorbing elements
- E04B1/8409—Sound-absorbing elements sheet-shaped
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- E04F—FINISHING WORK ON BUILDINGS, e.g. STAIRS, FLOORS
- E04F13/00—Coverings or linings, e.g. for walls or ceilings
- E04F13/002—Coverings or linings, e.g. for walls or ceilings made of webs, e.g. of fabrics, or wallpaper, used as coverings or linings
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- B32B2307/10—Properties of the layers or laminate having particular acoustical properties
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- B32—LAYERED PRODUCTS
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- B32B2607/00—Walls, panels
- B32B2607/02—Wall papers, wall coverings
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- C08J2323/00—Characterised by the use of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Derivatives of such polymers
- C08J2323/02—Characterised by the use of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Derivatives of such polymers not modified by chemical after treatment
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Abstract
The invention relates to a sound-absorbing and sound-insulating multilayer film, a composite structure thereof, wallpaper and a preparation method thereof, wherein the multilayer film comprises a first surface film and a second surface film, and the thickness of the first surface film and the second surface film is respectively 10-15 mu m; the foam hole core layer is positioned between the first surface layer film and the second surface layer film, and the thickness of the foam hole core layer is 30-50 mu m; the cell core layer comprises the following raw material components in percentage by weight: 85-94% of matrix resin, 0.2-2% of antioxidant, 0.2-2% of lubricating dispersant, 0.03-5% of pore-forming agent, 0-7% of compatilizer and 0-5% of chain extender. The ultrathin sound-absorbing and sound-insulating multilayer film is prepared by coextrusion and biaxial stretching, has the single thickness of only 60-80 microns, but has the sound-absorbing coefficient of more than 0.2 and the sound-insulating capability of more than 80dB, and realizes the light and thin continuous production of the sound-absorbing and sound-insulating material. The pattern layer is applied on the outermost layer of the composite structure containing the multilayer film, so that wallpaper can be directly produced, and home decoration integration is realized.
Description
Technical Field
The invention belongs to the field of sound-absorbing and sound-insulating composite materials, and particularly relates to a sound-absorbing and sound-insulating multilayer film and a composite structure thereof, wallpaper comprising the composite structure and a preparation method thereof.
Background
Noise pollution, water pollution and air pollution are called as three main pollution in the current society, and prevention and isolation of noise pollution are one of hot topics in the current society. The sources of noise are mainly traffic noise, industrial noise, construction noise and social life noise. Prolonged exposure to noisy environments increases the risk of deafness, diabetes and myocardial infarction. According to the characteristics of reflection, absorption and the like of sound waves in the propagation process, the noise treatment mode mainly comprises sound absorption and sound insulation.
The sound absorption means that the sound absorption material or the sound absorption structure is utilized to absorb and consume the incident sound energy, and the reflected sound is reduced, thereby reducing the noise. At present, most of sound absorbing materials are microporous sound absorbing structures, when sound waves are incident on the porous sound absorbing materials, due to viscous resistance of air, vibration friction between the air and hole walls is caused, so that a considerable part of sound energy is converted into heat energy to be absorbed, and the sound absorbing materials are called material sound absorption.
The sound insulation material plays an indispensable role in life and production, and aims to reduce the transmission of sound, make the sound difficult to pass through, isolate noise pollution and achieve the effects of protecting hearing and maintaining physical and psychological health.
The development of sound absorbing and insulating materials has also undergone decades of new generations, ranging from original sound absorbing cotton, wood and concrete boards to present multi-layer composites, whose properties have changed over the sky. In terms of the current usage, many modified sound absorbing cotton is used in home decoration. The current sound absorbing cotton mainly comprises a porous inner core and a hard surface, and is mainly used in the fields of indoor home decoration, factory soundproof rooms and the like. The developed pore structure can effectively reflect the incident sound wave to ensure that the incident sound wave is lost, meanwhile, the material has higher damping, the energy of the sound wave can be absorbed through oscillation, the effect of double sound absorption and noise reduction is achieved, and the sound absorption coefficient can generally reach 0.6 or even higher.
For sound insulation materials, according to the law of mass, the heavier the material (the greater the density or mass per unit area), the better the sound insulation effect, and good sound insulation materials tend to be very dense and also require to block the various gaps that can transmit sound. In addition, the disadvantage of the sound-absorbing cotton as a common sound-absorbing material is quite obvious, the volume of the sound-absorbing cotton is large due to the existence of very high porosity, too much installation space is occupied in home decoration, and the sound-absorbing effect is reduced once the installation volume of the sound-absorbing cotton is reduced, so that the light and thin home decoration design requirement is difficult to meet. Another limiting factor is that the sound-absorbing and sound-insulating material is poor in production continuity, and is generally produced by a discontinuous hot-pressing lamination mode or a mode of producing a foaming core layer by extrusion and then producing a hard surface layer by composite gluing, so that the production cost is high, and the mass production and popularization difficulty is high.
Patent CN112497858B discloses a composite board and a processing method thereof, which can obtain a composite board with higher sound absorption coefficient, wider sound absorption frequency band, higher structural strength and longer service life, and has simple processing technology and low production cost. The composite sound absorption board comprises a base board, a glue layer and a film layer, wherein the thickness of the base board is 0.2-15mm, a plurality of through holes penetrating through the thickness direction are formed in the base board, and the equivalent hydraulic diameter of the through holes is not less than 1.0mm; the film layer is adhered to the substrate through the adhesive layer and covers the through hole; and a gap is formed at the position of the film layer corresponding to the through hole. Compared with the traditional suction sound insulation board, the invention has the advantages that the overall thickness is reduced, but the substrate is still thick and heavy, the film layer structure is single, the requirement of high sound absorption and insulation performance under unit volume can not be met, and the continuous production mode is difficult to be adopted, so that the large-scale batch production is not facilitated.
Patent application CN112669800a provides a film-porous material composite structure with high-efficiency sound absorption performance, which consists of a porous material substrate and a film attached and fixedly connected to one end face of the porous material substrate. The thickness of the sound-absorbing material is thin, which is 1/8-1/10 of the thickness of the sound-absorbing material used in the current industry, and the sound-absorbing material has high-efficiency sound-absorbing performance; and the film and the porous material are combined to realize the diversity of the porous material structure and effectively improve the broadband sound absorption performance of the porous material. However, the composite structure of the invention is relatively complex, is difficult to realize low-cost continuous industrial production, and cannot meet the huge consumption of markets such as building, decoration and the like.
Patent CN105835497B discloses a preparation method of intelligent heat-insulating sound-insulating PVB film, the intelligent heat-insulating sound-insulating PVB film includes first PVB layer, second sound-insulating layer and third PVB layer that connect gradually, includes following step: (1) Adding vanadium dioxide nano powder into alcohol to dissolve to form a VO 2 solution, blending the VO 2 solution with resin powder to obtain a second sound-insulating layer master batch, and processing the second sound-insulating layer master batch into a second sound-insulating layer containing a three-dimensional channel structure functional layer; (2) And blending the second sound insulation layer with PVB resin powder, and performing coextrusion or roll forming to obtain the intelligent heat-insulating sound-insulating PVB film. Through adopting 3D to print or lithographically formed three-dimensional channel structure and not to the damping realization sound insulation effect, integrate sound insulation and thermal-insulated performance simultaneously on the PVB rete, form the novel PVB intermediate layer that has thermal-insulated sound insulation function, and thickness is 0.38mm, 0.76mm or 1.14mm one of them. Although the three-layer composite structure is continuously formed by adopting a coextrusion mode, the overall thickness of the interlayer film is still thicker, and the preparation means of the sound insulation layer is complex, the production cost is high, and the high-efficiency mass production is difficult.
On the other hand, the requirements of high-quality indoor decoration are increasingly outstanding at any time when the living standard of people is improved, the existing sound-absorbing and sound-insulating material is generally a plate, and is mostly fixed by rivets and the like in the home decoration process, and is only used as a concealed structural material, and the exterior of the sound-absorbing and sound-insulating material still needs to be adhered with surface decoration such as wallpaper, emulsion paint and the like, and cannot be subjected to integrated repair design, so that the defects of complex decoration materials, complicated construction procedures, increased pollution risk and the like are caused.
Therefore, how to provide a multilayer film and a composite structure thereof which are excellent in sound absorption and insulation properties and convenient for lamination design, and to expand the uses of the multilayer film and the composite structure and to increase the added value thereof, is a technical problem to be solved in the art.
Disclosure of Invention
Aiming at the defects in the prior art, the invention aims to provide the sound-absorbing and sound-insulating multilayer film, the composite structure thereof, the wallpaper comprising the composite structure and the preparation method, so as to provide the multilayer film with excellent sound-absorbing and sound-insulating performance and convenient lamination design and the composite structure thereof, and the wallpaper with high added value is prepared efficiently and at low cost by applying pattern design on the outermost layer of the composite structure, thereby improving the use convenience of the sound-absorbing and sound-insulating material, reducing construction procedures and pollution links and lowering cost.
Specifically, the invention provides a sound-absorbing and sound-insulating multilayer film, which comprises the following components:
the thickness of the first surface layer film and the second surface layer film is 10-15 mu m respectively;
the foam hole core layer is positioned between the first surface layer film and the second surface layer film, and the thickness of the foam hole core layer is 30-50 mu m;
the foam cell core layer comprises the following raw material components in percentage by weight:
the multilayer film is prepared by melt coextrusion and biaxial stretching, and has a sound absorption coefficient of more than 0.2 and a sound insulation capacity of more than 80 dB.
The three-layer composite film is designed by simulating the traditional sound-absorbing cotton structure through the coextrusion and biaxially oriented ABA film method, has a harder surface layer structure and a porous core layer structure, and can provide a good sound-absorbing and sound-insulating effect. And the ultra-thin thickness of the micron level ensures that the device has larger adaptability and designability, and realizes the goals of light weight, thinness and popularization.
For the specific selection of the raw material types of the foam cell core layer, the matrix resin is at least one of PETG, LDPE and copolymer PP, TPE, PA. The matrix resin with low crystallinity is selected, so that the core layer has higher toughness, thereby providing sufficient damping and sound absorption effects and being beneficial to improving the sound absorption effect of the sound absorption and insulation multilayer film. In addition, the corresponding compatibilizer may be selected according to the kind of matrix resin, for example, when copolymerized PP is selected as the matrix resin, at least one of PP-g-MAH, PP-g-GMA may be selected. The use of the compatilizer establishes a bridge effect for the compatible combination of the core layer and the surface layer from the resin layer surface, improves the interlayer peeling strength, and is beneficial to prolonging the service life of the product.
Similarly, a suitable lubricating dispersant may be selected according to the characteristics of the matrix resin, and is preferably at least one of erucamide, EBS, PETS, and calcium stearate. On one hand, the lubricating and dispersing agent provides external lubrication for the matrix resin to enable the matrix resin to flow smoothly in the screw and the cylinder, and on the other hand, the lubricating and dispersing agent is beneficial to uniformly dispersing auxiliaries such as pore-forming agents and the like in the machine body.
The antioxidant can be compounded by one or more of 1098, 1076, 168 and 626 which are commonly used in the field.
The chain extender is preferably 4,4' -di-sec-butylamino-diphenyl-methane, the content of which is 0.5-1.5%. The use of the chain extender can lead the matrix resin to generate chain extension and crosslinking reaction, thereby being beneficial to increasing the melt strength and preventing the collapse and the rupture of the holes.
The pore-forming agent is at least one of hollow glass beads, a foaming agent and a stretching pore-forming agent.
Preferably, the pore-forming agent comprises 1-5% of hollow glass beads, the particle size of the hollow glass beads is 3-5 mu m, and the hollow glass beads are modified by a silane coupling agent, and the pore-forming agent comprises the following steps:
Step one: preparing an ethanol solution of a silane coupling agent with the mass fraction of 1-3%, preparing the ethanol solution to pH of 5-5.5 by using a hydrochloric acid solution with the mass fraction of 2-5%, and stirring the mixture for 5-10min to obtain a modified solution;
step two: dispersing the hollow glass beads in the modified solution by ultrasonic waves, and standing for 60-80min;
Step three: taking out and baking for 80-100min at 120-130 ℃ to obtain the hollow glass microsphere modified by the silane coupling agent.
The blowing agent may be selected from organic and/or inorganic blowing agents commonly used in the art, such as ammonium chloride blowing agents, azodicarbonamide (AC) blowing agents, oxo-bis-benzenesulfonyl hydrazide blowing agents, supercritical gas blowing agents (e.g., carbon dioxide, nitrogen, air, etc.), and the like, with ammonium chloride being preferred. The foaming agent is used for processing a screw extruder, a large number of holes are formed in matrix resin after the foaming agent is heated and decomposed, and volatile matters are released into foam materials after the matrix is cooled. In view of the fact that closed cell structures generally have better sound absorption capacity than open cell structures, on one hand, a small amount of foaming agent is added to avoid the occurrence of thin cell wall and a large amount of perforated structures, and the cross-linking enhancement effect of the chain extender is added to enable the cell wall to have larger thickness and strength; on the other hand, based on the co-extrusion molding method, in the cooling stage after extrusion, the volatile matters are difficult to fully release due to the constraint of the matrix resin and the surface layer film, and can only be cooled to become solid to cause volume shrinkage, but the pore walls have enough thickness and strength, so that the pores can not completely collapse, and a hole similar to a vacuum state is formed, so that a better sound absorption effect is achieved.
Stretching pore-forming agents, which mainly utilize the crystal structure of the matrix resin, form many pores when subjected to stress, and are commonly used in dry production of porous films. Taking the copolymerized PP matrix resin as an example, a large amount of beta crystals are generated on the PP substrate through the beta nucleating agent, and the beta crystals are hexagonal crystals, so that a large amount of pores are generated when the PP substrate is subjected to tensile stress.
Further, the cell core layer further comprises 1-5% of modified polyacrylonitrile nanofiber, and the diameter of the modified polyacrylonitrile nanofiber is 150-250nm, and the modified polyacrylonitrile nanofiber is prepared by the following method:
step one: preparing 10-20% of spinning solution by using polyacrylonitrile particles and N, N-dimethylformamide, and adding the spinning solution into electrostatic spinning equipment to obtain polyacrylonitrile nanofiber; preferably, the spinning solution is magnetically stirred for 10 to 12 hours under the heat preservation condition of 50 to 60 ℃ to obtain a fully dissolved and uniformly dispersed solution;
Step two: and (3) ultrasonically dispersing the polyacrylonitrile nanofiber in a solution of 3-8% of cyano silane coupling agent, performing surface treatment for 2-4h at 50-80 ℃, and cooling and filtering to obtain the modified polyacrylonitrile nanofiber.
The addition of the nanofiber can help to improve the strength of the core layer, provide a more stable structural foundation for the diffusion, conversion and absorption of sound waves in the material and provide conditions for reducing the overall thickness of the core layer and the multilayer film; on the other hand, the nanofiber has a specific surface area and a porosity which are 1000-10000 times higher than those of common fibers, and the acting area of sound waves and fibers is increased, so that the nanofiber also has the capabilities of resonance sound absorption and porous sound absorption.
The polyacrylonitrile nanofiber adopted by the invention has a higher melting point, can resist the high temperature effect of the technological process of coextrusion and the like, and is subjected to surface modification treatment of the cyano silane coupling agent, so that the dispersion uniformity and compatibility of the nanofiber in matrix resin are further improved, and the core layer with excellent sound absorption performance can be obtained.
Besides the special design of the core layer, the invention has good sound absorption performance, and the sound insulation performance of the two surface films is also particularly concerned, so that the sound absorption and insulation performance of the multilayer film is integrally improved.
Preferably, the first surface layer film and the second surface layer film respectively comprise the following raw material components in percentage by weight:
For the specific selection of the raw material types of the surface film, the antioxidant preferably comprises a main antioxidant and an auxiliary antioxidant, the main antioxidant can be hindered phenols commonly used in the field, such as 1098 and 1076 of An Long, and the main function of the main antioxidant is to reduce free radicals generated by cracking of the resin after oxidation into peroxides, so that the aim of preventing chain reaction is fulfilled, but the peroxides can be further subjected to homolytic reaction under high temperature or ultraviolet conditions to generate free radicals, so that the auxiliary antioxidant also needs to be added, and the auxiliary antioxidant can be selected from phosphite esters and thioesters commonly used in the field, such as 168 and DSTP, and the auxiliary antioxidant can reduce the peroxides into carboxylic acids, so that the homolytic reaction is prevented from generating free radicals to initiate oxidative cleavage reaction. The ratio of the amounts of primary and secondary antioxidants can be determined based on the actual situation, e.g., the ratio of the available functional groups of the raw materials.
The lubricating dispersant may be correspondingly configured according to the selected resin characteristics, for example, at least one selected from erucamide, EBS, PETS.
The nucleating agent, at least one of nano inorganic particles and glycol ester nucleating agents, mainly provides heterogeneous nucleation points, and provides a foundation for rapidly forming a large number of crystal nuclei for the surface layer, so that the crystallization degree of the surface layer material is increased by the crystal growth through the later shaping section, the surface density of the surface layer material is improved to achieve the purpose of reflecting sound waves, and the sound insulation performance of the material is improved. For the nano inorganic particles, at least one of nano BaSO4 and nano SiO2 is preferable. Ethylene glycol ester nucleating agents, such as TegMeR 809, have good water resistance and low temperature properties, and act as nucleating agents in thermoplastics such as PET, lower Tg of the plastics, and enable processing speed to be faster and temperature to be lower.
The opening agent is mainly composed of micron-sized inorganic particles and is used for preventing the film from adhering during winding.
The color master batch is used for adjusting the color of a product and preferably comprises 60-70% of PET resin substrate and 30-40% of toner in percentage by weight.
Further, the first skin layer film and the second skin layer film may be different in composition, and the first skin layer film or the second skin layer film further comprises 0.4-3% of ultrafine glass fibers in percentage by weight, wherein the diameter of the ultrafine glass fibers is less than 5 μm, and the length-diameter ratio is 3:1 to 5:1, the method is processed and obtained by the following steps:
step one: drying chopped glass fiber with diameter below 5 μm at 400-500 deg.C;
step two: milling for a certain period of time by using a planetary ball mill, and sieving to obtain the length-diameter ratio of 3:1 to 5:1, ultra-fine glass fiber;
Step three: carrying out surface treatment on the superfine glass fiber by adopting plasma, wherein the treatment conditions are as follows: vacuum degree is 3×10 -3-5×10-3 mmHg, carrier gas is 50% N 2 and 50% CF 4, treatment power is 150-250W, and treatment time is 3-5min.
The addition of the superfine glass fiber can enhance the added surface layer film on one hand, and on the other hand, the superfine glass fiber can easily form bonding points on the surface of the surface layer film according to the thickness of the surface layer film and the size of the glass fiber, and can extend into matrix resin of the core layer to provide mechanical anchoring effect in the process of coextrusion bonding, so that the interlayer bonding strength is further improved. In addition, the ultra fine glass fiber is added only in one of the first surface layer film and the second surface layer film so that the surface layer film to which the ultra fine glass fiber is not added is the outermost layer of the product, so that patterning such as printing is smoothly performed. Of course, depending on the location of use of the multilayer film, for example, it is not necessary to provide a patterned skin layer, but only as a laminated interlayer, it is also optional to add ultra fine glass fibers to both skin films to improve mechanical properties and peel strength.
The interfacial bonding strength of the microglass fibers with the resin is generally relatively low, and improvement of the matrix resin properties is limited. Many methods for treating the surface of the fiber are preferred, and from the viewpoints of simplification of the process, environmental protection, stability, etc., the surface treatment of the fiber with plasma is preferred. The plasma collides with the surface of the fiber material to break chemical bonds on the surface part of the fiber material to form free radicals with high chemical activity, so that new chemical bonds are formed, the polarity and chemical reactivity of the surface of the fiber material are enhanced, and the interfacial compatibility of the fiber material is improved, so that the composite material with better interfacial compatibility and more remarkable enhancement effect is obtained. In addition, the invention particularly uses the mixed reaction gas of N 2 and CF 4, and the gas CF 4 has mild etching effect and extremely strong fluorination property, and can introduce fluorine-containing functional groups on the surface of the fiber, thereby further reducing the surface energy of the material. The plasma modification treatment has the advantages of simple operation, short treatment time, stable quality and small material performance loss.
The ABA (or ABA') ultrathin sound-absorbing and sound-insulating multilayer film is prepared by coextrusion and biaxial stretching, has the single thickness of only 60-80 microns, but has the sound-absorbing coefficient of more than 0.2 and the sound-insulating capability of more than 80dB, and realizes the light, thin and continuous production of sound-absorbing and sound-insulating materials.
The invention further provides a composite structure which is formed by bonding at least two sound-absorbing and sound-insulating multilayer films, and an adhesive layer with the thickness of 5-10 mu m is further arranged between the adjacent multilayer films; the adhesive layer comprises the following components in percentage by weight:
Wherein the adhesive resin is at least one selected from epoxy resin, EVA hot melt adhesive, polyurethane, polyamide and EEA; the resin is a bonding resin commonly used in the field, and the corresponding curing agent and curing accelerator are selected according to the selected bonding resin; the hollow glass beads can be the same as those in the core layer.
The sound-absorbing and sound-insulating multilayer film provided by the invention has the micron-sized thickness, more than 6 combined layers can be easily achieved by bonding two or more films, the limit of the thickness to the layers is effectively broken, the total thickness of the film is not more than 1mm even if 10 films are bonded, the upper limit of the layers is higher, the degree of freedom regulation is large, and the design range of sound-absorbing and sound-insulating performance is wide.
In addition, after coextrusion biaxial stretching, lamination to obtain the composite structure can be continuously produced, and the production efficiency is high and the cost is low. For specific layers and modes, when the number of layers to be laminated is small, for example, less than 5 layers, 5 layers of films can be unreeled and laminated at one time to obtain a composite structure; if more films are laminated, the lamination mode of gradually superposing layers is preferable to reduce equipment requirements and ensure lamination quality.
In particular, when the ultra fine glass fiber is added to one of the first skin film and the second skin film, the skin film to which the ultra fine glass fiber is not added is used as the outermost layer of the product, and the skin film to which the ultra fine glass fiber is added is combined with the adhesive layer and laminated in order to obtain a desired thickness and sound absorption and insulation effects. Similar to the combination of the surface film and the core layer, the surface film added with the superfine glass fiber and the adhesive layer also form a mechanical anchoring effect, so that the interlayer combination strength is improved.
In order to further expand the application and added value of the sound-absorbing and sound-insulating multilayer film and the composite structure thereof, the invention further provides wallpaper, which comprises the composite structure and a pattern layer applied on the outermost layer of the composite structure.
The pattern layer can form the wallpaper with various colors, concave-convex stereo and other private custom-made and independent style designs through various means such as ink printing, 3D printing and the like, and also can realize low-cost mass production of the wallpaper, simplify home decoration design and reduce hidden troubles such as adhesive pollution attached to the traditional wallpaper.
Correspondingly, the invention also provides a preparation method of the wallpaper, which comprises the following steps:
step one: preparing sound-absorbing and sound-insulating multilayer film
S1.1: respectively feeding the raw materials of the first surface layer film, the second surface layer film and the foam cell core layer into three extruders, and carrying out melt coextrusion; and electrostatically adsorbing the molten steel to a cooling roller to cool the molten steel into a casting sheet; specific preferred includes the following steps:
S1.1.1, respectively adding the three layers of raw materials into a high-speed stirrer for mixing at the rotating speed of 500-600r/min for 15-20min, metering the raw materials by a metering scale after uniformly mixing, and adding the raw materials into an extruder;
S1.1.2 extruding raw materials at 200-280 ℃ by a main machine for a foam core layer and two auxiliary machines for a surface layer membrane, pressurizing by a melt pump, and passing through a 12-micro-pore-diameter filter, wherein the temperature of the filter is set to 240-280 ℃;
S1.1.3 melt enters a three-layer co-extrusion die head after passing through a T-shaped frame, the temperature of the die head is 200-220 ℃, and the thickness ratio of each layer in the film is regulated and controlled by controlling the ratio of the melt extruded by a main machine and an auxiliary machine;
S1.1.4 the co-extrusion lamellar matter is electrostatically adsorbed on a cooling roller to form a casting sheet, the electrostatic voltage is 10-15kV, the thickness of the casting sheet is controlled to be 150-850 mu m, the rotating speed of the cooling roller is 18-35m/min, and the temperature of the cooling roller is 25-32 ℃;
s1.2: biaxially stretching the cast sheet to obtain a biaxially stretched film; specific preferred includes the following steps:
S1.2.1: stretching in the longitudinal direction
Preheating at 70-80deg.C, cooling at 20-30deg.C, and longitudinal stretching at 30-50deg.C; the longitudinal stretching multiplying power is 2-4 times;
S1.2.2: transverse stretching
Preheating at 95-105deg.C, stretching at 105-115 deg.C, heat setting at 110-120 deg.C, and cooling at 30-60deg.C; the transverse stretching multiplying power is 3-5 times.
S1.3: carrying out double-sided corona treatment on the biaxially oriented film to form a corona layer; after static electricity is removed, rolling to obtain a sound absorption and insulation multilayer film; wherein the thickness of the first surface layer film and the second surface layer film is 10-15 μm respectively, the thickness of the cell core layer is 30-50 μm, and the total thickness is preferably 75-80 μm;
step two: preparation of composite structures
S2.1: unreeling at least two sound-absorbing and sound-insulating multilayer films, and coating an adhesive on the surface to be laminated of the multilayer films; preferably, the coating line preheating temperature is 70-90 ℃, implemented by a preheating roller set;
s2.2: laminating the multilayer films and curing the adhesive to form an adhesive layer between adjacent multilayer films; preferably, the curing temperature is 90-100 ℃, implemented by a curing roller set;
s2.3: cooling, removing static electricity and rolling to obtain the composite structure; preferably, the cooling temperature is 30-50 ℃, the cooling is implemented by a cooling roller, and the rolling action is implemented by a rolling roller;
A plurality of the multi-layer films can be adhered and laminated according to the thickness, the sound absorption and insulation performance and the like, so that a required composite structure is obtained; when the number of to-be-laminated is small, for example, less than 5 sheets, 5 sheets of multi-layer films can be unreeled and laminated at one time to obtain a composite structure; if more films are laminated, the lamination mode of gradually superposing layers is preferable to reduce equipment requirements and ensure lamination quality.
Step three: and applying a pattern layer on the outermost layer of the composite structure, and cutting to obtain the wallpaper.
The invention has the advantages that:
1. The ABA (or ABA') type ultrathin sound-absorbing and sound-insulating film is prepared by adopting the raw materials of the cellular core layer and the surface layer with reasonable composition and proportion through coextrusion and biaxial stretching, has the single thickness of 60-80 microns, but has the sound-absorbing coefficient of more than 0.2 and the sound-insulating capability of more than 80dB, meets the basic requirements of sound-absorbing and sound-insulating materials (the sound-insulating standard of building materials such as houses, study and the like usually needs to meet more than 45dB, see the sound-insulating design Specification of civil buildings (GB 50118-2010), and the material with the sound-absorbing coefficient exceeding 0.2 can be called as the sound-absorbing material), and realizes the light, thin and continuous production of the sound-absorbing and sound-insulating material.
2. The composite structure is prepared by bonding a plurality of films, the thickness regulation degree is large, and the design range of sound absorption and insulation performance is wide. Taking 10 films as an example, the total thickness is less than 1mm, but the sound absorption coefficient can reach 0.8 or more, the sound insulation can reach 118dB or more, and the sound absorption and insulation capability is excellent.
3. The production efficiency is high, the production of the film with the width of 6 meters per minute can reach more than 30 meters, and the continuous automatic operation production can be realized.
4. The double surfaces subjected to corona can be subjected to operations such as electroplating color ink printing, coating adhesion and the like, so that the operation procedures are reduced, the pollution risk is reduced, and the home decoration integration is realized efficiently.
Drawings
The above, as well as additional purposes, features, and advantages of exemplary embodiments of the present disclosure will become readily apparent from the following detailed description when read in conjunction with the accompanying drawings. Several embodiments of the present disclosure are illustrated by way of example, and not by way of limitation, in the figures of the accompanying drawings and in which like reference numerals refer to similar or corresponding parts and in which:
FIG. 1 is a schematic view of a sound absorbing and insulating multilayer film of the present invention;
FIG. 2 is a schematic illustration of a composite structure of the present invention;
fig. 3 is a schematic view of the lamination process of the composite structure of the present invention.
Reference numerals illustrate: 1. the foam core layer, the first surface layer film, the second surface layer film, the corona layer and the adhesive layer are respectively arranged in the cavity of the foam core layer, the first surface layer film, the second surface layer film, the corona layer and the adhesive layer 3.1 preheating roller set, 3.2 solidifying roller set, 3.3 cooling roller, 3.4 point measuring type coating device 3.5 hollow glass bead sprayer, 100 sound absorption and insulation multilayer film, 101 first unreeling roller, 102 second unreeling roller, 103 wind-up roller, 200 composite structure.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention will be further described in detail with reference to the accompanying drawings.
The sound-absorbing and sound-insulating multilayer film 100 of the present invention comprises:
The thickness of the first surface film 2 and the second surface film 3 is 10-15 mu m respectively;
The foam hole core layer 1 is positioned between the first surface layer film 2 and the second surface layer film 3, and has the thickness of 30-50 mu m;
The foam cell core layer 1 comprises the following raw material components in percentage by weight:
The first surface layer film 2 and the second surface layer film 3 respectively comprise the following raw material components:
the multilayer film is prepared by melt coextrusion and biaxial stretching, and has a sound absorption coefficient of more than 0.2 and a sound insulation capacity of more than 80 dB.
In the foam cell core layer 1, the matrix resin is at least one of PETG, LDPE and copolymer PP, TPE, PA. The antioxidant can be compounded by one or more of 1098, 1076, 168 and 626 which are commonly used in the field. The lubricating dispersant is at least one of erucamide, EBS, PETS and calcium stearate. The chain extender is preferably 4,4' -di-sec-butylamino-diphenyl-methane, the content of which is 0.5-1.5%. When the copolymerized PP is selected as the matrix resin, the compatilizer is at least one of PP-g-MAH and PP-g-GMA. The pore-forming agent is at least one of hollow glass beads, a foaming agent and a stretching pore-forming agent.
The blowing agent may be selected from organic and/or inorganic blowing agents commonly used in the art, such as ammonium chloride blowing agents, azodicarbonamide (AC) blowing agents, oxo-bis-benzenesulfonyl hydrazide blowing agents, supercritical gas blowing agents (e.g., carbon dioxide, nitrogen, air, etc.), and the like, with ammonium chloride being preferred.
The hollow glass microsphere used in the pore-forming agent has the content of 1-5wt% and the particle diameter of 3-5 mu m, and is modified by the silane coupling agent, comprising the following steps:
Step one: preparing an ethanol solution of a silane coupling agent with the mass fraction of 1-3%, preparing the ethanol solution to pH of 5-5.5 by using a hydrochloric acid solution with the mass fraction of 2-5%, and stirring the mixture for 5-10min to obtain a modified solution;
step two: dispersing the hollow glass beads in the modified solution by ultrasonic waves, and standing for 60-80min;
Step three: taking out and baking for 80-100min at 120-130 ℃ to obtain the hollow glass microsphere modified by the silane coupling agent.
The cell core layer 1 also comprises 1-5% of modified polyacrylonitrile nano-fiber with the diameter of 150-250nm, and the modified polyacrylonitrile nano-fiber is prepared by the following method:
Step one: preparing 10-20% of spinning solution by using polyacrylonitrile particles and N, N-dimethylformamide, and adding the spinning solution into electrostatic spinning equipment to obtain polyacrylonitrile nanofiber; the spinning solution is magnetically stirred for 10 to 12 hours under the heat preservation condition of 50 to 60 ℃ to obtain a fully dissolved and uniformly dispersed solution;
Step two: and (3) ultrasonically dispersing the polyacrylonitrile nanofiber in a solution of 3-8% of cyano silane coupling agent, performing surface treatment for 2-4h at 50-80 ℃, and cooling and filtering to obtain the modified polyacrylonitrile nanofiber.
In the first surface film 2 and the second surface film 3, the antioxidant preferably comprises a primary antioxidant and a secondary antioxidant, wherein the primary antioxidant can be hindered phenols commonly used in the field, such as 1098, 1076 and the like of An Long; the secondary antioxidant may be selected from phosphite esters, thioesters commonly used in the art, such as 168, DSTP, etc.
The lubricating dispersant may be correspondingly configured according to the selected resin characteristics, for example, at least one selected from erucamide, EBS, PETS.
The nucleating agent is at least one of nano inorganic particles and glycol ester nucleating agents. As the nano inorganic particles, at least one of nano BaSO 4 and nano SiO 2 is preferable. As the ethylene glycol ester nucleating agent, tegMeR 809,809 can be selected.
The opening agent is mainly composed of micron-sized inorganic particles and is used for preventing the film from adhering during winding.
The color master batch comprises 60-70% of PET resin substrate and 30-40% of toner by weight percent.
The first surface film 2 or the second surface film 3 further comprises 0.4-3% of ultra-fine glass fibers, wherein the diameter of the ultra-fine glass fibers is less than 5 μm, and the length-diameter ratio is 3:1 to 5:1, the method is processed and obtained by the following steps:
step one: drying chopped glass fiber with diameter below 5 μm at 400-500 deg.C;
step two: milling for a certain period of time by using a planetary ball mill, and sieving to obtain the length-diameter ratio of 3:1 to 5:1, ultra-fine glass fiber;
Step three: carrying out surface treatment on the superfine glass fiber by adopting plasma, wherein the treatment conditions are as follows: vacuum degree is 3×10 -3-5×10-3 mmHg, carrier gas is 50% N 2 and 50% CF 4, treatment power is 150-250W, and treatment time is 3-5min.
The composite structure 200 of the present invention is formed by bonding at least two of the above sound-absorbing and sound-insulating multilayer films 100, and further comprises an adhesive layer 5 having a thickness of 5-10 μm between adjacent ones of the multilayer films; the adhesive layer 5 comprises the following components in percentage by weight:
Wherein the adhesive resin is at least one selected from epoxy resin, EVA hot melt adhesive, polyurethane, polyamide and EEA; the resin is a bonding resin commonly used in the field, and the corresponding curing agent and curing accelerator are selected according to the selected bonding resin; the hollow glass beads can be the same as those in the core layer.
When the ultra fine glass fiber is added to one of the first and second skin films 2 and 3, the skin film to which the ultra fine glass fiber is not added is taken as the outermost layer of the product, and the skin film to which the ultra fine glass fiber is added is combined with the adhesive layer 5 and laminated in order to obtain a desired thickness and sound absorption and insulation effect, for example, 5, 8, 10 or more of the multilayer films are laminated to obtain the composite structure 200.
The wallpaper of the present invention comprises the composite structure 200, and a pattern layer applied on the outermost layer of the composite structure 200.
The pattern layer can form the wallpaper with various colors, concave-convex stereo and other private custom-made and independent style designs through various means such as ink printing, 3D printing and the like, and also can realize low-cost mass production of the wallpaper, simplify home decoration design and reduce hidden troubles such as adhesive pollution attached to the traditional wallpaper.
Correspondingly, the preparation method of the wallpaper provided by the invention comprises the following steps:
step one: preparation of Sound absorbing and insulating multilayer film 100
S1.1 co-extrusion and preparation of cast sheet:
S1.1.1, respectively adding the three layers of raw materials into a high-speed stirrer for mixing at the rotating speed of 500-600r/min for 15-20min, metering the raw materials by a metering scale after uniformly mixing, and adding the raw materials into an extruder;
S1.1.2 extruding raw materials at 200-280 ℃ by a main machine for a foam core layer 1 and two auxiliary machines for a surface layer film, pressurizing by a melt pump, and passing through a 12-15-micrometer pore-size filter, wherein the temperature of the filter is set to 240-280 ℃;
S1.1.3 melt enters a three-layer co-extrusion die head after passing through a T-shaped frame, the temperature of the die head is 200-220 ℃, and the thickness ratio of each layer in the film is regulated and controlled by controlling the ratio of the melt extruded by a main machine and an auxiliary machine;
s1.1.4 the co-extrusion lamellar matter is electrostatically adsorbed on a cooling roller 3.3 to form a casting sheet, the electrostatic voltage is 10-15kV, the thickness of the casting sheet is controlled to be 150-850 mu m, the rotating speed of the cooling roller 3.3 is 18-35m/min, and the temperature of the cooling roller 3.3 is 25-32 ℃;
s1.2: biaxially stretching the cast sheet to obtain a biaxially stretched film:
S1.2.1: stretching in the longitudinal direction
Preheating at 70-80deg.C, cooling at 20-30deg.C, and longitudinal stretching at 30-50deg.C; the longitudinal stretching multiplying power is 2-4 times;
S1.2.2: transverse stretching
Preheating at 95-105deg.C, stretching at 105-115 deg.C, heat setting at 110-120 deg.C, and cooling at 30-60deg.C; the transverse stretching multiplying power is 3-5 times.
S1.3: carrying out double-sided corona treatment on the biaxially oriented film to form a corona layer 4; after static electricity is removed, rolling to obtain the sound-absorbing and sound-insulating multilayer film 100; wherein the thickness of the first surface layer film 2 and the second surface layer film 3 is 10-15 μm respectively, the thickness of the foam core layer 1 is 30-50 μm, and the total thickness is preferably 75-80 μm;
Step two: preparation of composite Structure 200
S2.1: unreeling at least two sound-absorbing and sound-insulating multilayer films 100, and coating an adhesive on the surface to be laminated of the multilayer films; preferably, taking two multi-layer films 100 as an example, unreeling by using a first unreeling roller 101 and a second unreeling roller 102, wherein the preheating temperature of a coating line is 70-90 ℃, the coating is implemented by a preheating roller set 3.1, and the coating of the adhesive is implemented by using a spot-type coater 3.4 and a hollow glass bead sprayer 3.5 together;
s2.2: laminating the multilayer films and curing the adhesive to form an adhesive layer 5 between adjacent multilayer films; preferably, the curing temperature is 90-100 ℃, implemented by a curing roller set 3.2;
S2.3: cooling, removing static electricity and rolling to obtain the composite structure 200; preferably, the cooling temperature is 30-50 ℃, the cooling is implemented by a cooling roller 3.3, and the winding action is completed by a winding roller 103;
Laminating a plurality of the multilayer films according to the thickness, sound absorption and insulation properties and the like to obtain a desired composite structure 200, preferably laminating 5 or more, more preferably 10 or more; for specific layers and modes, when the number of layers to be laminated is small, for example, less than 5 sheets, 5 sheets of multi-layer films can be unreeled and laminated at one time to obtain the composite structure 200; if more films are laminated, the lamination mode of gradually superposing layers is preferable to reduce equipment requirements and ensure lamination quality.
Step three: and (3) applying a pattern layer on the outermost layer of the composite structure 200, and cutting to obtain the wallpaper.
Example 1:
(1) The formula comprises the following components:
(1.1) cell core layer 1:
Matrix resin: korean LG film-grade co-PP (brand T3450M), weight ratio 90%;
An antioxidant: li Anlong 1076 to 1076 weight percent of 0.2 percent and 168 weight percent of 0.1 percent of compound;
Lubricating and dispersing agent: erucamide, weight ratio is 0.3%;
Pore-forming agent: hollow glass beads (K20, grain size 5 μm, 3M Co., USA) 5% by weight, modified with a silane coupling agent;
And (3) a compatilizer: PP-g-MAH (DuPont 50E806, U.S.A.), 2% by weight;
chain extender: 4,4' -di-sec-butylaminodiphenyl methane (trade name Unilink 4200-MDBA) 0.4% by weight;
the polyacrylonitrile nanofiber has the diameter of 180+/-20 nm and the weight ratio of 2 percent, and is modified by a cyano silane coupling agent.
(1.2) First top film 2:
Resin: constant-escape bright film-grade PET resin with 67% by weight; producing recycled materials, wherein the weight ratio is 30%;
An antioxidant: li Anlong 1076 to 1076 weight percent of 0.2 percent and 168 weight percent of 0.1 percent of compound;
Lubricating and dispersing agent: pentaerythritol stearate (PETS), weight ratio 0.4%;
nucleating agent: tegMeR 809A 809, 1% by weight
And (3) an opening agent: 1, 6-hexanediol diglycidyl ether, 0.6% by weight;
Color master batch: 0.7% by weight; based on 100 percent of the total weight of the color master batch, the color master batch comprises 60 to 70 percent of constant-escape large bright film grade PET resin and 30 to 40 percent of toner.
(1.3) Second top film 3:
Resin: constant-escape large bright film grade PET resin with the weight ratio of 66 percent; producing recycled materials, wherein the weight ratio is 30%;
An antioxidant: li Anlong 1076 to 1076 weight percent of 0.2 percent and 168 weight percent of 0.1 percent of compound;
lubricating and dispersing agent: pentaerythritol stearate (PETS), weight ratio 0.6%;
nucleating agent: tegMeR 809A 809, 1% by weight;
And (3) an opening agent: 1, 6-hexanediol diglycidyl ether, 0.6% by weight;
Superfine glass fiber: 1.5% by weight, and plasma surface-treated.
(1.4) Adhesive layer 5
Adhesive resin: the weight ratio of the epoxy resin, the curing agent, the curing accelerator and the hollow glass beads (K20 of 3M company of America, particle size 5 μm) is 1:0.75:0.05:0.05.
(2) Process and parameters
Step one: preparation of Sound absorbing and insulating multilayer film 100
S1.1 co-extrusion and preparation of cast sheet:
S1.1.1, respectively adding the three layers of raw materials into a high-speed stirrer for mixing at the rotating speed of 500-600r/min for 15-20min, metering the raw materials by a metering scale after uniformly mixing, and adding the raw materials into an extruder;
S1.1.2 a main machine for the foam core layer 1 extrudes raw materials at 200-260 ℃, two auxiliary machines for the surface layer film extrude the raw materials at 200-240 ℃, the raw materials are pressurized by a melt pump, and the raw materials pass through a 15-micrometer pore-size filter, wherein the temperature of the filter is set to 240-260 ℃;
S1.1.3 after passing through a T-shaped frame, the melt enters a three-layer co-extrusion die head, the temperature of the die head is 200 ℃, and the auxiliary machine 1 is controlled: and (3) a host computer: the extruded melt ratio of the auxiliary machine 2 was 16:68:16 to regulate the thickness ratio of each layer in the film;
s1.1.4 the coextruded lamellar matter is electrostatically adsorbed on a cooling roller 3.3 to form a casting sheet, the electrostatic voltage is 10kV, the thickness of the casting sheet is 675 mu m, the rotating speed of the cooling roller 3.3 is 26m/min, and the temperature of the cooling roller 3.3 is 30 ℃;
s1.2: biaxially stretching the cast sheet to obtain a biaxially stretched film:
S1.2.1: stretching in the longitudinal direction
The preheating temperature is 70 ℃, 74, 76 and 77 ℃ in sequence, the cooling temperature is 28 ℃, and the longitudinal drawing shaping temperature is 35 and 45 ℃ in sequence; the longitudinal stretching multiplying power is 3.2 times;
S1.2.2: transverse stretching
The preheating temperature is 90, 95, 100 and 105 ℃ in sequence, the stretching temperature is 105, 110 and 115 ℃ in sequence, the heat setting temperature is 110, 115 and 120 ℃ in sequence, and the cooling temperature is 30, 45 and 60 ℃ in sequence; the transverse stretching ratio was 3.2 times.
S1.3: carrying out double-sided corona treatment on the biaxially oriented film to form a corona layer 4; after static electricity is removed, rolling to obtain the sound-absorbing and sound-insulating multilayer film 100; wherein the thickness of the first surface layer film 2 and the second surface layer film 3 is 11+/-1 mu m respectively, the thickness of the foam hole core layer 1 is 52+/-2 mu m, and the total thickness is about 75 mu m; the sound absorption coefficient was measured to be 0.40 and the sound insulation was measured to be 115dB.
Step two: preparation of composite Structure 200
S2.1: unwinding 2 sheets of the sound-absorbing and sound-insulating multilayer film 100, and coating an adhesive on the surface to be laminated of the multilayer film, wherein the unit coating amount is 20g/m 2; the preheating temperature of the preheating roller set 3.1 on the coating line is 70, 75 and 80 ℃ in sequence;
S2.2: laminating the multilayer films and curing the adhesive to form an adhesive layer 5 between adjacent multilayer films, the thickness being about 5 μm; the curing temperature of the curing roller set 3.2 is 90, 95 and 100 ℃ in sequence;
S2.3: the cooling roller 3.3 is used for cooling and removing static electricity, and the intermediate structure is obtained by winding through the winding roller 103; the cooling temperature is 35 ℃;
repeating the steps S2.1-S2.3, and laminating 10 multi-layer films in a layer-by-layer lamination mode, wherein the surface layer film, the cell core layer 1, the surface layer film and the bonding layer 5 are sequentially and circularly laminated, 39 layers are added in total, the sound absorption coefficient is 0.88, and the sound insulation is 150dB;
step three: and spraying and painting on the upper surface of the outermost layer of the composite structure 200, and cutting to obtain wallpaper.
Example 2:
example 2 differs from example 1 in that the composition of the second top film 3 is different, and this example does not contain ultra fine glass fibers, i.e., the first top film 2 and the second top film 3 have the same composition.
The first surface film 2 and the second surface film 3 each contain the following raw material components:
Resin: constant-escape bright film-grade PET resin with 67% by weight; producing recycled materials, wherein the weight ratio is 30%;
An antioxidant: li Anlong 1076 to 1076 weight percent of 0.2 percent and 168 weight percent of 0.1 percent of compound;
Lubricating and dispersing agent: pentaerythritol stearate (PETS), weight ratio 0.4%;
nucleating agent: tegMeR 809A 809, 1% by weight
And (3) an opening agent: 1, 6-hexanediol diglycidyl ether, 0.6% by weight;
Color master batch: 0.7% by weight; based on 100 percent of the total weight of the color master batch, the color master batch comprises 60 to 70 percent of constant-escape large bright film grade PET resin and 30 to 40 percent of toner.
The multilayer film produced had: the thickness of the first surface layer film 2 and the second surface layer film 3 is 11+/-1 mu m, the thickness of the foam core layer 1 is 52+/-2 mu m, and the total thickness is about 75 mu m; the sound absorption coefficient was tested to be 0.4 and the sound insulation was tested to be 95dB.
The composite structure 200 is obtained by laminating 10 multi-layer films, wherein a surface layer film, a cell core layer 1, a surface layer film and an adhesive layer 5 are sequentially and circularly laminated, 39 layers are added in total, the sound absorption coefficient is 0.82, and the sound insulation is 120dB.
Example 3:
Example 3 differs from example 2 mainly in that the pore former in the cell core layer 1 of this example is an ammonium chloride blowing agent.
(1.1) Cell core layer 1:
matrix resin: korean LG film-grade co-PP (trade mark T3450M), 92% by weight;
An antioxidant: li Anlong 1076 to 1076 weight percent of 0.2 percent and 168 weight percent of 0.1 percent of compound;
Lubricating and dispersing agent: erucamide, weight ratio is 0.3%;
pore-forming agent: ammonium chloride, 3% by weight;
And (3) a compatilizer: PP-g-MAH (DuPont 50E806, U.S.A.), 2% by weight;
chain extender: 4,4' -di-sec-butylaminodiphenyl methane (trade name Unilink 4200-MDBA) 0.4% by weight;
the polyacrylonitrile nanofiber has the diameter of 180+/-20 nm and the weight ratio of 2 percent, and is modified by a cyano silane coupling agent.
The multilayer film produced had: the thickness of the first surface layer film 2 and the second surface layer film 3 is 11+/-1 mu m, the thickness of the foam core layer 1 is 52+/-2 mu m, and the total thickness is about 75 mu m; the sound absorption coefficient was measured to be 0.30 and the sound insulation was measured to be 110dB.
The composite structure 200 is obtained by laminating 10 multi-layer films, wherein a surface layer film, a cell core layer 1, a surface layer film and an adhesive layer 5 are sequentially and circularly laminated, 39 layers are total, the sound absorption coefficient is 0.90, and the sound insulation is 139dB.
Example 4:
(1) The formula comprises the following components:
(1.1) cell core layer 1:
matrix resin: korean LG film-grade co-PP (trade mark T3450M), 92% by weight;
An antioxidant: li Anlong 1076 to 1076 weight percent of 0.2 percent and 168 weight percent of 0.1 percent of compound;
Lubricating and dispersing agent: erucamide, weight ratio is 0.3%;
Pore-forming agent: hollow glass beads (K20, grain size 5 μm, 3M Co., USA) 5% by weight, modified with a silane coupling agent;
And (3) a compatilizer: PP-g-MAH (DuPont 50E806, U.S.A.), 2% by weight;
Chain extender: 4,4' -bis-sec-butylaminodiphenyl methane (trade name Unilink 4200-MDBA) 0.4% by weight.
(1.2) The first skin layer film 2 and the second skin layer film 3 each contain:
Resin: constant-escape bright film-grade PET resin with 67% by weight; producing recycled materials, wherein the weight ratio is 30%;
An antioxidant: li Anlong 1076 to 1076 weight percent of 0.2 percent and 168 weight percent of 0.1 percent of compound;
Lubricating and dispersing agent: pentaerythritol stearate (PETS), weight ratio 0.4%;
nucleating agent: tegMeR 809A 809, 1% by weight
And (3) an opening agent: 1, 6-hexanediol diglycidyl ether, 0.6% by weight;
Color master batch: 0.7% by weight; based on 100 percent of the total weight of the color master batch, the color master batch comprises 60 to 70 percent of constant-escape large bright film grade PET resin and 30 to 40 percent of toner.
(1.3) Adhesive layer 5
Adhesive resin: the weight ratio of the epoxy resin, the curing agent, the curing accelerator and the hollow glass beads (K20 of 3M company of America, particle size 5 μm) is 1:0.75:0.05:0.05.
(3) Process and parameters
Step one: preparation of Sound absorbing and insulating multilayer film 100
S1.1 co-extrusion and preparation of cast sheet:
S1.1.1, respectively adding the three layers of raw materials into a high-speed stirrer for mixing at the rotating speed of 500-600r/min for 15-20min, metering the raw materials by a metering scale after uniformly mixing, and adding the raw materials into an extruder;
S1.1.2 a main machine for the foam core layer 1 extrudes raw materials at 200-260 ℃, two auxiliary machines for the surface layer film extrude the raw materials at 200-240 ℃, the raw materials are pressurized by a melt pump, and the raw materials pass through a 15-micrometer pore-size filter, wherein the temperature of the filter is set to 240-260 ℃;
S1.1.3 after passing through a T-shaped frame, the melt enters a three-layer co-extrusion die head, the temperature of the die head is 200 ℃, and the auxiliary machine 1 is controlled: and (3) a host computer: the extruded melt ratio of the auxiliary machine 2 was 18:64:18, regulating and controlling the thickness ratio of each layer in the film;
S1.1.4 the coextrusion lamellar matter is electrostatically adsorbed onto a cooling roller 3.3 to form a casting sheet, the electrostatic voltage is 10kV, the thickness of the casting sheet is 615 mu m, the rotating speed of the cooling roller 3.3 is 26m/min, and the temperature of the cooling roller 3.3 is 30 ℃;
s1.2: biaxially stretching the cast sheet to obtain a biaxially stretched film:
S1.2.1: stretching in the longitudinal direction
The preheating temperature is 70 ℃, 74, 76 and 77 ℃ in sequence, the cooling temperature is 28 ℃, and the longitudinal drawing shaping temperature is 35 and 45 ℃ in sequence; the longitudinal stretching multiplying power is 3.2 times;
S1.2.2: transverse stretching
The preheating temperature is 90, 95, 100 and 105 ℃ in sequence, the stretching temperature is 105, 110 and 115 ℃ in sequence, the heat setting temperature is 110, 115 and 120 ℃ in sequence, and the cooling temperature is 30, 45 and 60 ℃ in sequence; the transverse stretching ratio was 3.2 times.
S1.3: carrying out double-sided corona treatment on the biaxially oriented film to form a corona layer 4; after static electricity is removed, rolling to obtain the sound-absorbing and sound-insulating multilayer film 100; wherein the thickness of the first surface layer film 2 and the second surface layer film 3 is 11+/-1 mu m respectively, the thickness of the foam hole core layer 1 is 42+/-2 mu m, and the total thickness is about 65 mu m; the sound absorption coefficient was measured to be 0.20 and the sound insulation was measured to be 80dB.
Step two: preparation of composite Structure 200
S2.1: unwinding 2 sheets of the sound-absorbing and sound-insulating multilayer film 100, and coating an adhesive on the surface to be laminated of the multilayer film, wherein the unit coating amount is 20g/m 2; the preheating temperature of the preheating roller set 3.1 on the coating line is sequentially 70, 75 and 80 ℃;
S2.2: laminating the multilayer films and curing the adhesive to form an adhesive layer 5 between adjacent multilayer films, the thickness being about 5 μm; the curing temperature of the curing roller set 3.2 is 90, 95 and 100 ℃ in sequence;
S2.3: the cooling roller 3.3 is used for cooling, removing static electricity and winding through the winding roller 103 to obtain the composite structure 200; the cooling temperature is 35 ℃;
Repeating the steps S2.1-S2.3, and laminating 10 multi-layer films in a layer-by-layer lamination mode, wherein the surface layer film, the cell core layer 1, the surface layer film and the bonding layer 5 are sequentially and circularly laminated, 39 layers are added in total, the sound absorption coefficient is 0.80, and the sound insulation is 118dB;
step three: and spraying and painting on the upper surface of the outermost layer of the composite structure 200, and cutting to obtain wallpaper.
Example 5:
(1) The formula comprises the following components:
(1.1) cell core layer 1:
matrix resin: PA6 (japan part 1013B), weight ratio 94%;
An antioxidant: li Anlong 1076 to 1076 weight percent of 0.2 percent and 168 weight percent of 0.1 percent of compound;
lubricating and dispersing agent: PETS, weight ratio 0.3%;
Pore-forming agent: stretching pore-forming agent (brand Baolimei CL-50) with a weight ratio of 5%;
Chain extender: 4,4' -bis-sec-butylaminodiphenyl methane (trade name Unilink 4200-MDBA) 0.4% by weight.
(1.2) The first skin layer film 2 and the second skin layer film 3 each contain:
Resin: constant-escape bright film-grade PET resin with 67% by weight; producing recycled materials, wherein the weight ratio is 30%;
An antioxidant: li Anlong 1076 to 1076 weight percent of 0.2 percent and 168 weight percent of 0.1 percent of compound;
Lubricating and dispersing agent: pentaerythritol stearate (PETS), weight ratio 0.4%;
nucleating agent: tegMeR 809A 809, 1% by weight
And (3) an opening agent: 1, 6-hexanediol diglycidyl ether, 0.6% by weight;
Color master batch: 0.7% by weight; based on 100 percent of the total weight of the color master batch, the color master batch comprises 60 to 70 percent of constant-escape large bright film grade PET resin and 30 to 40 percent of toner.
(1.3) Adhesive layer 5
Adhesive resin: the weight ratio of the epoxy resin, the curing agent, the curing accelerator and the hollow glass beads (K20 of 3M company of America, particle size 5 μm) is 1:0.75:0.05:0.05.
(4) Process and parameters
Step one: preparation of Sound absorbing and insulating multilayer film 100
S1.1 co-extrusion and preparation of cast sheet:
S1.1.1, respectively adding the three layers of raw materials into a high-speed stirrer for mixing at the rotating speed of 500-600r/min for 15-20min, metering the raw materials by a metering scale after uniformly mixing, and adding the raw materials into an extruder;
S1.1.2 a main machine for the foam core layer 1 extrudes raw materials at 240-275 ℃, two auxiliary machines for the surface layer film extrude the raw materials at 200-240 ℃, the raw materials are pressurized by a melt pump, and the raw materials pass through a 15-micrometer pore-size filter, wherein the temperature of the filter is set to 240-280 ℃;
S1.1.3 after passing through a T-shaped frame, the melt enters a three-layer co-extrusion die head, the temperature of the die head is 200 ℃, and the auxiliary machine 1 is controlled: and (3) a host computer: the extruded melt ratio of the auxiliary machine 2 was 16:68:16 to regulate the thickness ratio of each layer in the film;
S1.1.4 the coextruded lamellar matter is electrostatically adsorbed on a cooling roller 3.3 to form a casting sheet, the electrostatic voltage is 10kV, the thickness of the casting sheet is 675 mu m, the rotating speed of the cooling roller 3.3 is 30m/min, and the temperature of the cooling roller 3.3 is 30 ℃;
s1.2: biaxially stretching the cast sheet to obtain a biaxially stretched film:
S1.2.1: stretching in the longitudinal direction
The preheating temperature is 70 ℃, 74, 76 and 77 ℃ in sequence, the cooling temperature is 28 ℃, and the longitudinal drawing shaping temperature is 35 and 45 ℃ in sequence; the longitudinal stretching multiplying power is 3.2 times;
S1.2.2: transverse stretching
The preheating temperature is 90, 95, 100 and 105 ℃ in sequence, the stretching temperature is 105, 110 and 115 ℃ in sequence, the heat setting temperature is 110, 115 and 120 ℃ in sequence, and the cooling temperature is 30, 45 and 60 ℃ in sequence; the transverse stretching ratio was 3.2 times.
S1.3: carrying out double-sided corona treatment on the biaxially oriented film to form a corona layer 4; after static electricity is removed, rolling to obtain the sound-absorbing and sound-insulating multilayer film 100; wherein the thickness of the first surface layer film 2 and the second surface layer film 3 is 11+/-1 mu m respectively, the thickness of the foam hole core layer 1 is 52+/-2 mu m, and the total thickness is about 75 mu m; the sound absorption coefficient was measured to be 0.21 and the sound insulation was measured to be 122dB.
Step two: preparation of composite Structure 200
S2.1: unwinding 2 sheets of the sound-absorbing and sound-insulating multilayer film 100, and coating an adhesive on the surface to be laminated of the multilayer film, wherein the unit coating amount is 20g/m 2; the preheating temperature of the preheating roller set 3.1 on the coating line is sequentially 70, 75 and 80 ℃;
s2.2: laminating the multilayer films and curing the adhesive to form an adhesive layer 5 between adjacent multilayer films, the thickness being about 5 μm; the curing temperature of the curing roller set 3.2 is 90, 95 and 100 ℃ in sequence;
S2.3: the cooling roller 3.3 is used for cooling, removing static electricity and winding through the winding roller 103 to obtain the composite structure 200; the cooling temperature is 35 ℃;
Repeating the steps S2.1-S2.3, and laminating 10 multi-layer films in a layer-by-layer lamination mode, wherein the surface layer film, the cell core layer 1, the surface layer film and the bonding layer 5 are sequentially and circularly laminated, 39 layers are added in total, the sound absorption coefficient is 0.9, and the sound insulation is 155dB;
step three: and spraying and painting on the upper surface of the outermost layer of the composite structure 200, and cutting to obtain wallpaper.
Table 1 shows the parameters related to the multilayer films and the composite structures of examples 1-5
The single thickness of the multilayer film is only 60-80 microns, but the multilayer film has the sound absorption coefficient of more than 0.2 and the sound insulation capacity of more than 80dB, and the basic requirements of the sound absorption and insulation material are met; when the composite structure is prepared by lamination, the sound absorption coefficient of the corresponding composite structure is above 0.80, and part of embodiments can reach 0.90, and the sound insulation coefficient is correspondingly improved, so that the composite structure meets the standard of excellent sound absorption and insulation materials (the sound absorption coefficient is above 0.5, the sound insulation coefficient is above 55dB and the sound absorption and insulation performance is good). In addition, the composite member of the embodiment of the invention is obtained by laminating 10 multi-layer films, the thickness of the composite member is not more than 1mm, if the sound absorption and insulation effects are further improved, even if the lamination number is continuously increased, the thickness of the composite member has a quite large competitive advantage, and the composite member is strong in designability and simple to operate.
In addition to the good sound absorption and insulation properties, the embodiment 1 with the surface layer containing the superfine glass fibers has relatively good mechanical properties, and is more beneficial to the long-term use of the sound absorption and insulation material. Examples 1-3, which contain nanofibers in the cellular core, have good overall properties, particularly sound absorption and insulation properties of their composite structures.
Example 4 has relatively low sound absorption and insulation performance before and after lamination due to the overall thickness, particularly the small thickness of the cell core layer, but can also meet the daily sound absorption and insulation requirements.
In example 3, a foaming agent was used, and in example 5, a stretched pore-forming agent was used, and although the sound absorption performance of the single multilayer film was relatively insignificant, the sound absorption performance of the laminated composite member was significantly improved, which may be related to a good composite member composite pore size and pore-forming uniformity.
In the whole, the multilayer film and the composite member thereof have the mechanical properties which are obviously improved compared with the common sound-absorbing and sound-insulating materials in the prior art, such as foam plates (the tensile strength is usually about 30 MPa) and the like, so that the use stability and the service life are improved, and the use scene is widened.
The foregoing description of the preferred embodiments of the present invention has been presented for purposes of clarity and understanding, and is not intended to limit the invention to the particular embodiments disclosed, but is intended to cover all modifications, alternatives, and improvements within the spirit and scope of the invention as outlined by the appended claims.
Claims (9)
1. A sound absorbing and insulating multilayer film comprising:
the thickness of the first surface layer film and the second surface layer film is 10-15 mu m respectively;
the foam hole core layer is positioned between the first surface layer film and the second surface layer film, and the thickness of the foam hole core layer is 30-50 mu m;
the foam cell core layer comprises the following raw material components in percentage by weight:
85-94% of matrix resin
Antioxidant 0.2-2%
0.2 To 2 percent of lubricating dispersant
Pore-forming agent 0.03-5%
0 To 7 percent of compatilizer
0-5% Of chain extender;
The multilayer film is prepared by melt coextrusion and biaxial stretching, and has a sound absorption coefficient of more than 0.2 and a sound insulation capacity of more than 80 dB;
the pore-forming agent is at least one of hollow glass beads, a foaming agent and a stretching pore-forming agent;
the cell core layer also comprises 1-5% of modified polyacrylonitrile nano-fiber with the diameter of 150-250nm, and the modified polyacrylonitrile nano-fiber is prepared by the following method:
Step one: preparing 10-20% of spinning solution by using polyacrylonitrile particles and N, N-dimethylformamide, and adding the spinning solution into electrostatic spinning equipment to obtain polyacrylonitrile nanofiber;
Step two: and (3) ultrasonically dispersing the polyacrylonitrile nanofiber in a solution of 3-8% of cyano silane coupling agent, performing surface treatment for 2-4h at 50-80 ℃, and cooling and filtering to obtain the modified polyacrylonitrile nanofiber.
2. The multilayer film of claim 1, wherein the matrix resin is at least one of PETG, LDPE, co-polymer PP, TPE, PA; the lubricating dispersant is at least one of erucamide, EBS, PETS and calcium stearate.
3. The multilayer film of claim 2, wherein the pore-forming agent comprises 1-5% by weight of hollow glass microspheres having a particle size of 3-5 μm and a wall thickness of 0.2-1 μm, and is modified with a silane coupling agent, comprising the steps of:
Step one: preparing an ethanol solution of a silane coupling agent with the mass fraction of 1-3%, preparing the ethanol solution to the pH of 5-5.5 by using a hydrochloric acid solution with the mass fraction of 2-5%, and stirring the mixture for 5-10min to obtain a modified solution;
step two: dispersing the hollow glass beads in the modified solution by ultrasonic waves, and standing for 60-80min;
Step three: taking out and baking for 80-100min at 120-130 ℃ to obtain the hollow glass microsphere modified by the silane coupling agent.
4. A multilayer film according to any one of claims 1 to 3, wherein the first and second skin films each comprise the following raw material components in weight percent:
90-99% of PET resin or PA resin
Antioxidant 0.2-2%
0.2 To 2 percent of lubricating dispersant
0.2 To 2 percent of nucleating agent
0 To 2 percent of opening agent
0-3% Of color master batch.
5. The multilayer film of claim 4, wherein the first skin layer film or the second skin layer film further comprises 0.4-3% by weight of ultra fine glass fibers having a diameter of 5 μm or less and an aspect ratio of 3:1 to 5:1, the method is processed and obtained by the following steps:
step one: drying chopped glass fiber with diameter below 5 μm at 400-500 deg.C;
step two: milling for a certain period of time by using a planetary ball mill, and sieving to obtain the length-diameter ratio of 3:1 to 5:1, ultra-fine glass fiber;
Step three: carrying out surface treatment on the superfine glass fiber by adopting plasma, wherein the treatment conditions are as follows: vacuum degree is 3×10 -3-5×10-3 mmHg, carrier gas is 50% N 2 and 50% CF 4, treatment power is 150-250W, and treatment time is 3-5min.
6. A composite structure formed by bonding at least two sound-absorbing and insulating multilayer films according to any one of claims 1 to 5, characterized in that between adjacent ones of said multilayer films, an adhesive layer having a thickness of 5 to 10 μm is included; the adhesive layer comprises the following components in percentage by weight:
52-56% of adhesive resin
39-42% Of curing agent
1-5% Of curing accelerator
0-5% Of hollow glass beads.
7. A wallpaper comprising the composite structure of claim 6, and a patterned layer applied over an outermost layer of the composite structure.
8. A method of making wallpaper according to claim 7, comprising the steps of:
step one: preparing sound-absorbing and sound-insulating multilayer film
S1.1: respectively feeding the raw materials of the first surface layer film, the second surface layer film and the foam cell core layer into three extruders, and carrying out melt coextrusion; and electrostatically adsorbing the molten steel to a cooling roller to cool the molten steel into a casting sheet;
s1.2: biaxially stretching the cast sheet to obtain a biaxially stretched film;
S1.3: carrying out double-sided corona treatment on the biaxially oriented film; after static electricity is removed, rolling to obtain a sound absorption and insulation multilayer film;
step two: preparation of composite structures
S2.1: unreeling at least two sound-absorbing and sound-insulating multilayer films, and coating an adhesive on the surface to be laminated of the multilayer films;
s2.2: laminating the multilayer films and curing the adhesive to form an adhesive layer between adjacent multilayer films;
S2.3: cooling, removing static electricity and rolling to obtain the composite structure;
step three: and applying a pattern layer on the outermost layer of the composite structure to obtain the wallpaper.
9. The method of claim 8, wherein in step S1.2, biaxially stretching the cast sheet comprises the steps of:
S1.2.1: stretching in the longitudinal direction
Preheating at 70-80deg.C, cooling at 20-30deg.C, and longitudinal stretching at 30-50deg.C; the longitudinal stretching multiplying power is 2-4;
S1.2.2: transverse stretching
Preheating at 95-105deg.C, stretching at 105-115 deg.C, heat setting at 110-120 deg.C, and cooling at 30-60deg.C; the transverse stretching multiplying power is 3-5 times.
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