CN115521514B - Rubber compound, rubber layer, damping structure and preparation method thereof - Google Patents

Rubber compound, rubber layer, damping structure and preparation method thereof Download PDF

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Publication number
CN115521514B
CN115521514B CN202211192130.0A CN202211192130A CN115521514B CN 115521514 B CN115521514 B CN 115521514B CN 202211192130 A CN202211192130 A CN 202211192130A CN 115521514 B CN115521514 B CN 115521514B
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parts
rubber
damping structure
layer
weight
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CN115521514A (en
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郝敏
涂春潮
任玉柱
郭瑞毅
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Beijing Aviation Materials Research Institute Co ltd
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Beijing Aviation Materials Research Institute Co ltd
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    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L7/00—Compositions of natural rubber
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B64—AIRCRAFT; AVIATION; COSMONAUTICS
    • B64C—AEROPLANES; HELICOPTERS
    • B64C1/00—Fuselages; Constructional features common to fuselages, wings, stabilising surfaces or the like
    • B64C1/40—Sound or heat insulation, e.g. using insulation blankets
    • 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
    • C09J7/00—Adhesives in the form of films or foils
    • C09J7/20—Adhesives in the form of films or foils characterised by their carriers
    • C09J7/29—Laminated material
    • 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
    • C09J7/00—Adhesives in the form of films or foils
    • C09J7/30—Adhesives in the form of films or foils characterised by the adhesive composition
    • C09J7/38—Pressure-sensitive adhesives [PSA]
    • C09J7/381—Pressure-sensitive adhesives [PSA] based on macromolecular compounds obtained by reactions involving only carbon-to-carbon unsaturated bonds
    • C09J7/385—Acrylic polymers
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00—Use of inorganic substances as compounding ingredients
    • C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
    • C08K3/20—Oxides; Hydroxides
    • C08K3/22—Oxides; Hydroxides of metals
    • C08K2003/2227—Oxides; Hydroxides of metals of aluminium
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2201/00—Properties
    • C08L2201/02—Flame or fire retardant/resistant
    • 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
    • C09J2301/00—Additional features of adhesives in the form of films or foils
    • C09J2301/10—Additional features of adhesives in the form of films or foils characterized by the structural features of the adhesive tape or sheet
    • C09J2301/12—Additional features of adhesives in the form of films or foils characterized by the structural features of the adhesive tape or sheet by the arrangement of layers
    • C09J2301/122—Additional features of adhesives in the form of films or foils characterized by the structural features of the adhesive tape or sheet by the arrangement of layers the adhesive layer being present only on one side of the carrier, e.g. single-sided adhesive tape
    • 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
    • C09J2301/00—Additional features of adhesives in the form of films or foils
    • C09J2301/10—Additional features of adhesives in the form of films or foils characterized by the structural features of the adhesive tape or sheet
    • C09J2301/16—Additional features of adhesives in the form of films or foils characterized by the structural features of the adhesive tape or sheet by the structure of the carrier layer
    • 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
    • C09J2301/00—Additional features of adhesives in the form of films or foils
    • C09J2301/30—Additional features of adhesives in the form of films or foils characterized by the chemical, physicochemical or physical properties of the adhesive or the carrier
    • C09J2301/302—Additional features of adhesives in the form of films or foils characterized by the chemical, physicochemical or physical properties of the adhesive or the carrier the adhesive being pressure-sensitive, i.e. tacky at temperatures inferior to 30°C

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Engineering & Computer Science (AREA)
  • Health & Medical Sciences (AREA)
  • Medicinal Chemistry (AREA)
  • Polymers & Plastics (AREA)
  • Mechanical Engineering (AREA)
  • Aviation & Aerospace Engineering (AREA)
  • Compositions Of Macromolecular Compounds (AREA)

Abstract

The invention relates to a rubber compound for a damping structure, which adopts a rubber compound system comprising natural rubber, brominated butyl rubber and butadiene rubber as rubber compound of a rubber layer in the damping structure. The invention widens the damping temperature range of the rubber layer, so that the rubber layer has excellent damping performance in a wide damping temperature range. In addition, the rubber layer can completely meet the requirement of the navigable standard on flame retardance by adding the proper type of flame retardant into the rubber compound and controlling the reasonable proportion of the flame retardant. The invention also relates to a rubber layer, a damping structure and a preparation method thereof.

Description

Rubber compound, rubber layer, damping structure and preparation method thereof
Technical Field
The invention relates to the technical field of aviation materials, in particular to a rubber compound for a damping structure, a rubber layer, a damping structure and a preparation method of the damping structure.
Background
The requirements of high economy and high safety of large civil aircraft make many related aerodynamic problems to be solved urgently, vibration and noise are one of aerodynamic problems which must be paid attention to in the development stage of large civil aircraft, and the internal vibration and noise of the aircraft influence the comfortable riding environment of the carrier, so that the international acceptance degree of the model of the large civil aircraft is determined. Through long-term researches and designs, aerodynamic noise, jet noise and turbine vibration are reduced as much as possible, and aircraft designers put more efforts on acoustic packages of cabin structures, such as skins, and vibration response and noise level of cabin walls can be effectively reduced through laying damping layers on inner surfaces of the cabin skins, so that the effects of isolating engine vibration and noise transmission are achieved. However, the damping temperature range of the existing damping layer product is narrower, and the damping performance is poor.
Disclosure of Invention
In order to overcome the problems existing in the prior art, the invention provides a rubber compound for a damping structure, which adopts a raw rubber system comprising natural rubber, brominated butyl rubber and butadiene rubber as raw rubber of a rubber layer in the damping structure. The glass transition temperature Tg of the natural rubber is within the range of minus 50 ℃ to minus 35 ℃, the glass transition temperature Tg of the brominated butyl rubber is within the range of minus 20 ℃ to minus 5 ℃, the effective damping temperature ranges of the two rubbers cover the temperature range of the inner surface of the skin of the aircraft in the flight process, and the brominated butyl rubber has excellent damping in the temperature range. However, at a temperature close to-50 ℃, the natural rubber can be changed from a high-elastic state to a glassy state, and the modulus of the natural rubber can be remarkably increased, so that the improvement of structural damping can be inhibited. Therefore, the inventor adds butadiene rubber into the rubber compound to stabilize the modulus of the raw rubber system, widens the damping temperature range of the rubber layer, and ensures that the rubber layer has excellent damping performance in a wide damping temperature range.
The rubber compound for the damping structure provided by the first aspect of the invention is mainly prepared from the following raw materials:
65-75 parts of natural rubber, 15-25 parts of brominated butyl rubber and 5-15 parts of butadiene rubber.
In some embodiments, the natural rubber may be present in an amount of 65 parts by weight, 66 parts by weight, 67 parts by weight, 68 parts by weight, 69 parts by weight, 70 parts by weight, 71 parts by weight, 72 parts by weight, 73 parts by weight, 74 parts by weight, or 75 parts by weight.
In some embodiments, the brominated butyl rubber may be present in an amount of 15 parts by weight, 16 parts by weight, 17 parts by weight, 18 parts by weight, 19 parts by weight, 20 parts by weight, 21 parts by weight, 22 parts by weight, 23 parts by weight, 24 parts by weight, or 25 parts by weight.
In some embodiments, the butadiene rubber may be present in an amount of 5, 6, 7, 8, 9, 10, 11, 12, 13, 14, or 15 parts by weight.
In some embodiments, the mass ratio of natural rubber, brominated butyl rubber, and butadiene rubber may be (6.8-7.2): (1.8-2.2): (0.8-1.2). Preferably, the mass ratio of natural rubber, brominated butyl rubber and butadiene rubber is 7:2:1.
In some embodiments, the raw materials used to form the mix may further comprise: 65-75 parts of a first flame retardant and 35-45 parts of a second flame retardant, wherein the first flame retardant is aluminum hydroxide, and the second flame retardant is antimony trioxide.
In some embodiments, the first flame retardant may be present in an amount of 65 parts by weight, 66 parts by weight, 67 parts by weight, 68 parts by weight, 69 parts by weight, 70 parts by weight, 71 parts by weight, 72 parts by weight, 73 parts by weight, 74 parts by weight, or 75 parts by weight.
In some embodiments, the second flame retardant may be present in an amount of 35 parts by weight, 36 parts by weight, 37 parts by weight, 38 parts by weight, 39 parts by weight, 40 parts by weight, 41 parts by weight, 42 parts by weight, 43 parts by weight, 44 parts by weight, or 45 parts by weight.
In some embodiments, the mass ratio of the first flame retardant to the second flame retardant may be (6.8-7.2): 3.8-4.2. Preferably, the mass ratio of the first flame retardant to the second flame retardant may be 7:4.
By adding proper type of flame retardant into the rubber compound and controlling the reasonable proportion of the flame retardant, the generated rubber layer can meet the requirement of the navigable standard on flame retardance. The functional and flame-retarding capabilities of the damping layer are determined by the interaction and the amount of the flame retardant among the rubber layers and the flame retardant and the raw rubber system and other fillers. Therefore, the selection and the amount of the flame retardant determine the flame retardant property of the damping structure. The invention adopts a combined system of aluminum hydroxide and antimony trioxide as flame retardant filler, has the most excellent flame retardant effect when the ratio of the aluminum hydroxide to the antimony trioxide is 70:40, and the two flame retardants are added into a raw rubber system, so that the damping structure product can completely meet the requirement of the navigable standard on flame retardance through the synergistic effect of the two flame retardants. In the prior art, 100-300 parts (per 100 parts of raw rubber) of flame retardant is added into the rubber layer to realize excellent flame retardant property, but the addition of a large amount of flame retardant filler can dilute the raw rubber content in the rubber layer, so that the mechanical property and damping property are reduced, and the technological property is also reduced. The invention overcomes the defects of the prior art, and ensures that the damping structure has excellent flame retardant property and damping property by adding proper amount of aluminum hydroxide and antimonous oxide.
In some embodiments, the raw materials used to form the mix may further comprise: 10-15 parts of reinforcing agent, 1-3 parts of first plasticizer, 8-10 parts of second plasticizer, 3-6 parts of active agent, 1-2 parts of anti-aging agent, 2-3 parts of accelerator and 2-3 parts of vulcanizing agent.
In some embodiments, the reinforcing agent may be present in an amount of 10 parts by weight, 11 parts by weight, 12 parts by weight, 13 parts by weight, 14 parts by weight, or 15 parts by weight.
In some embodiments, the first plasticizer may be present in an amount of 1 part by weight, 1.5 parts by weight, 2 parts by weight, 2.5 parts by weight, or 3 parts by weight.
In some embodiments, the second plasticizer may be present in an amount of 8 parts by weight, 8.5 parts by weight, 9 parts by weight, 9.5 parts by weight, or 10 parts by weight.
In some embodiments, the active agent may be present in an amount of 3 parts by weight, 3.5 parts by weight, 4 parts by weight, 4.5 parts by weight, 5 parts by weight, 5.5 parts by weight, or 6 parts by weight.
In some embodiments, the anti-aging agent may be present in an amount of 1 part by weight, 1.1 parts by weight, 1.2 parts by weight, 1.3 parts by weight, 1.4 parts by weight, 1.5 parts by weight, 1.6 parts by weight, 1.7 parts by weight, 1.8 parts by weight, 1.9 parts by weight, or 2 parts by weight.
In some embodiments, the accelerator may be present in an amount of 2 parts by weight, 2.1 parts by weight, 2.2 parts by weight, 2.3 parts by weight, 2.4 parts by weight, 2.5 parts by weight, 2.6 parts by weight, 2.7 parts by weight, 2.8 parts by weight, 2.9 parts by weight, or 3 parts by weight.
In some embodiments, the vulcanizing agent may be present in an amount of 2 parts by weight, 2.1 parts by weight, 2.2 parts by weight, 2.3 parts by weight, 2.4 parts by weight, 2.5 parts by weight, 2.6 parts by weight, 2.7 parts by weight, 2.8 parts by weight, 2.9 parts by weight, or 3 parts by weight.
In some embodiments, the reinforcing agent may be carbon black, such as carbon black under the designation N330 or N550.
In some embodiments, the first plasticizer may be stearic acid, such as stearic acid under the designation 1840 or 1841.
In some embodiments, the second plasticizer may be dioctyl sebacate.
In some embodiments, the active agent may be zinc oxide.
In some embodiments, the anti-aging agent may include one or more of quinoline polymers, imidazole polymers, and p-phenylenediamine polymers, preferably 2, 4-trimethyl-1, 2-dihydroquinoline polymers.
In some embodiments, the accelerator may comprise one or more of tetramethylthiurams, benzothiazoles, preferably 2-mercaptobenzothiazole.
In some embodiments, the vulcanizing agent may be sulfur.
In some embodiments, the rubber compound is mainly prepared from the following raw materials: 65-75 parts of natural rubber, 15-25 parts of brominated butyl rubber, 5-15 parts of butadiene rubber, 10-15 parts of reinforcing agent, 65-75 parts of first flame retardant, 35-45 parts of second flame retardant, 1-3 parts of first plasticizer, 8-10 parts of second plasticizer, 3-6 parts of active agent, 1-2 parts of anti-aging agent, 2-3 parts of accelerator and 2-3 parts of vulcanizing agent.
Preferably, the rubber compound is mainly prepared by mixing the following raw materials: 70 parts of natural rubber, 20 parts of brominated butyl rubber, 10 parts of butadiene rubber, 12 parts of reinforcing agent, 70 parts of first flame retardant, 40 parts of second flame retardant, 2 parts of first plasticizer, 10 parts of second plasticizer, 5 parts of activator, 1 part of anti-aging agent, 3 parts of accelerator and 3 parts of vulcanizing agent.
The preparation method of the rubber compound comprises the following steps:
mixing natural rubber, brominated butyl rubber and butadiene rubber, heating to 55-60 ℃, adding a plasticizer, a reinforcing agent and an active agent, mixing, heating to 65-70 ℃, adding (for example, adding the flame retardant and the anti-aging agent for multiple times), mixing, heating to 75-80 ℃, discharging after mixing, putting the mixture into a sheet (for example, putting the sheet into an open mill for 4-6 times), and airing for more than 2 hours to obtain a primary mixed film;
and (3) after the primary mixed film is passed through (for example, the film is passed through for 3-5 times in an open mill), adding a vulcanizing agent and an accelerator, and after the vulcanizing agent and the accelerator are completely mixed, feeding the film into the film, for example, the film is passed through for 6-8 times, so as to obtain the rubber compound.
In a second aspect the invention provides a rubber layer for a damping structure formed from the elastomeric compound of the first aspect of the invention.
A third aspect of the present invention provides a damping structure, comprising, in order from bottom to top: a pressure sensitive adhesive layer, a rubber layer according to the second aspect of the present invention, and a constraining layer.
In some embodiments, the constraining layer is an aluminum plate.
The pressure-sensitive adhesive layer is made of acrylic ester materials.
In some embodiments, the constraining layer has a length and width of no less than 500mm and a thickness of 0.2-1.0mm, such as 0.2mm, 0.3mm, 0.4mm, 0.5mm, 0.6mm, 0.7mm, 0.8mm, 0.9mm, 1.0mm, and preferably 0.5mm.
In some embodiments, the thickness of the rubber layer may be 0.3mm-2mm, such as 0.3mm, 0.4mm, 0.5mm, 0.6mm, 0.7mm, 0.8mm, 0.9mm, 1mm, 1.1mm, 1.2mm, 1.3mm, 1.4mm, 1.5mm, 1.6mm, 1.7mm, 1.8mm, 1.9mm, or 2mm, preferably 1.3mm.
In some embodiments, the pressure sensitive adhesive layer may have a thickness of 0.12mm to 0.16mm, for example, 0.12mm, 0.13mm, 0.14mm, 0.15mm, or 0.16mm.
The use temperature of the damping structure can be between 50 ℃ below zero and 30 ℃ below zero, and the optimal use temperature is between 40 ℃ below zero and 5 ℃ below zero.
The damping structure can be adhered to the surface of the cabin skin of the civil aircraft, and plays an effective role in vibration reduction and noise reduction.
When the thickness of the damping structure is 1.9 mm-2.0 mm (wherein the thickness of rubber is 1.3mm, the thickness of the constraint layer is 0.5mm, and the thickness of the pressure-sensitive adhesive layer is 0.14 mm), the sound insulation test is carried out before and after the typical piece of the skin with the specification of 1.2 x 1.2m is laid on the damping structure according to the specification of ASTM E2249, and the insertion loss at 1000Hz is not lower than 1dB. The test result shows that the invention has excellent sound insulation and noise reduction performance.
When the thickness of the damping layer structure of the present invention is 1.9mm to 2.0mm (wherein the thickness of the rubber is 1.3mm, the thickness of the constraining layer is 0.5mm, and the thickness of the pressure sensitive adhesive is 0.14 mm), the base beam is oil hardened steel or peer material according to the specifications of ASTM E756, the specifications are 280mm±1mm in length, 12.5mm±0.2mm in width, and 1.6mm±0.05mm in thickness, and the damping structure is adhered to the base beam for cantilever beam test. The damping loss factor of the damping structure is not less than 0.3 at 50 Hz-1000 Hz minus 40 ℃ to minus 20 ℃. The test results reflect that the invention has excellent damping and vibration-absorbing performance.
When the thickness of the damping structure of the present invention is 1.9mm to 2.0mm (wherein the thickness of the rubber is 1.3mm, the thickness of the constraining layer is 0.5mm, and the thickness of the pressure-sensitive adhesive is 0.14 mm), the damping structure was subjected to flame retardant performance test according to the regulations of the CCAR25 section (the 25 th section of civil aviation regulations in china), the test items including 12s vertical burning, smoke density, burning and flame spread, and the damping structure of the present invention passed the examination of 12s vertical burning, smoke density and burning and flame spread.
A fourth aspect of the present invention provides a method for manufacturing a damping structure, including the steps of:
preparing the rubber compound according to the first aspect of the invention into a rubber sheet;
preheating a die for forming a damping structure;
providing a constraint layer, and coating an adhesive on the constraint layer;
placing the coated restraint layer and the film in a reserved mould for vulcanization molding;
after vulcanization molding is finished, unloading the mold to take out a damping structure semi-finished product, wherein the damping structure semi-finished product comprises a constraint layer and a rubber layer; and
and forming a pressure-sensitive adhesive layer on the rubber layer to obtain the damping structure.
In some embodiments, the method of making the film comprises the steps of:
mixing all the components for preparing the rubber compound, and thinning the lower piece to obtain the rubber compound;
and (5) wrapping the rubber compound into a film.
In some embodiments, the method of making the film comprises the steps of:
mixing natural rubber, brominated butyl rubber and butadiene rubber, heating to 55-60 ℃, adding a plasticizer, a reinforcing agent and an active agent, mixing, heating to 65-70 ℃, adding (for example, adding the flame retardant and the anti-aging agent for multiple times), mixing, heating to 75-80 ℃, discharging after mixing, putting the mixture into a sheet (for example, putting the sheet into an open mill for 4-6 times), and airing for more than 2 hours to obtain a primary mixed film;
after the primary mixed film is thinned (for example, thinned for 3-5 times in an open mill), vulcanizing agent and accelerator are added, and after the vulcanizing agent and accelerator are completely mixed, the thinned (for example, thinned for 6-8 times) is subjected to sheet feeding to obtain a rubber compound;
the rubber compound is reworked and rolled into uniform films.
In some embodiments, the method of remilling the elastomeric compound and wrapping it into a uniform film comprises: setting the roller temperature of the four-roller rubber calender to be 50+/-5 ℃, adjusting the roller spacing and the cutter distance of the four-roller rubber calender, placing the obtained rubber compound on a double-roller rubber calender, back-refining until the rubber sheet is soft and smooth and flat in surface, placing the back-refined rubber compound at the rubber feeding position of the four-roller rubber calender, wrapping the rubber sheet into uniform rubber sheet, testing the thickness of the rubber sheet by using a thickness gauge, and re-adjusting the roller spacing and re-measuring the thickness until the thickness reaches the target thickness if the thickness is not within the target value range. After the surface of the film is leveled, a scraper can be used for blanking, and the obtained film and the isolation cloth are attached and placed on a rolling shaft for coiling.
In some embodiments, the film is cut into a size blank prior to placing the film in a mold.
In some embodiments, the constraining layer is an aluminum plate and the method of applying the adhesive comprises: cleaning an aluminum plate, airing, brushing primer on the aluminum plate, placing the aluminum plate into a gluing cabinet, setting the temperature of the gluing cabinet at 35+/-5 ℃, placing for 30-40 min, coating a layer of glue, placing the aluminum plate into the gluing cabinet, setting the temperature of the gluing cabinet at 35+/-5 ℃ and placing for 30-40 min.
In some embodiments, the mold for forming the damping structure includes a middle mold, an upper mold, and a lower mold, and the mold preheating includes: assembling a middle die, an upper die and a lower die for forming a damping structure together, placing the middle die, the upper die and the lower die on a lower die plate of a vulcanization molding machine, and setting the temperatures of the upper die plate and the lower die plate of the vulcanization molding machine to 145 ℃; and (3) carrying out mould preheating after the upper die plate and the lower die plate are matched, wherein the preheating time is not less than 30min.
In some embodiments, vulcanization molding comprises: opening the vulcanization molding machine, separating the upper die from the middle die, taking out the middle die, laying a coated constraint layer (such as an aluminum plate) in the lower die cavity, wherein the surface coated with the adhesive faces upwards, mounting the middle die on the lower die, then laying the blank (obtained by shearing the rubber compound) on the constraint layer, closing the vulcanization molding machine, and carrying out exhaust operation for 12-14 times; vulcanizing after the exhaust is completed, wherein the gauge pressure of vulcanizing pressure is set to 15 MPa+/-2 MPa, and vulcanizing time is 15 min+/-3 min.
In some embodiments, after removal of the semi-finished damping structure, excess glue at the edges of the semi-finished product may be removed (e.g., using a wallpaper knife). When the wallpaper knife is used, care should be taken to avoid the knife edge from scratching the rubber.
In some embodiments, the method of forming a pressure sensitive adhesive layer on the rubber layer includes: and (3) placing one surface of the damping structure semi-finished product with the rubber layer upwards into a laminating machine, completely attaching the acrylic pressure-sensitive adhesive on the rubber layer through the laminating machine, and cutting off redundant double-sided adhesive by the laminating machine.
Compared with the prior art, the invention has the beneficial effects that:
the invention provides a rubber compound for a damping structure, which adopts a rubber compound system comprising natural rubber, brominated butyl rubber and butadiene rubber as rubber compound of a rubber layer in the damping structure. The glass transition temperature Tg of the natural rubber is within the range of minus 50 ℃ to minus 35 ℃, the glass transition temperature Tg of the brominated butyl rubber is within the range of minus 20 ℃ to minus 5 ℃, the effective damping temperature ranges of the two rubbers cover the temperature range of the inner surface of the skin of the aircraft in the flight process, and the brominated butyl rubber has excellent damping in the temperature range. However, at a temperature close to-50 ℃, the natural rubber can be changed from a high-elastic state to a glassy state, and the modulus of the natural rubber can be remarkably increased, so that the improvement of structural damping can be inhibited. Therefore, the inventor adds butadiene rubber into the rubber compound to stabilize the modulus of the raw rubber system, widens the damping temperature range of the rubber layer, and ensures that the rubber layer has excellent damping performance in a wide damping temperature range.
In addition, the rubber layer can meet the requirement of the navigable standard on flame retardance by adding the proper type of flame retardant into the rubber compound and controlling the reasonable proportion of the flame retardant.
Detailed Description
In order to make the technical problems, technical schemes and beneficial effects to be solved more clear, the invention is further described in detail below with reference to specific embodiments. It should be understood that the specific embodiments described herein are for purposes of illustration only and are not intended to limit the scope of the invention.
Unless defined otherwise, technical terms used in the following examples have the same meaning as commonly understood by one of ordinary skill in the art to which the present invention pertains. The experimental reagents used in the following examples are all conventional biochemical reagents unless otherwise specified; the raw materials, instruments, equipment, etc. used in the following examples are all commercially available or available by existing methods; the dosage of the experimental reagent is the dosage of the reagent in the conventional experimental operation if no special description exists; the experimental methods are conventional methods unless otherwise specified. Unless otherwise indicated, the starting materials in the examples of the present application were all purchased commercially, with natural rubber from Allangaceae, and brominated butyl rubber and butadiene rubber from Beijing Yanshan division, a company of China petrochemical Co., ltd.
Preparation of the rubber mixtures
Example 1
The natural rubber, brominated butyl rubber and butadiene rubber and various fillers are weighed according to the following weight parts: 70 parts of natural rubber, 20 parts of brominated butyl rubber, 10 parts of butadiene rubber, 12 parts of carbon black, 70 parts of aluminum hydroxide, 40 parts of antimony trioxide, 2 parts of stearic acid, 10 parts of dioctyl sebacate, 5 parts of zinc oxide, 1 part of an anti-aging agent RD (2, 4-trimethyl-1, 2-dihydroquinoline polymer), 3 parts of an accelerator M (2-mercaptobenzothiazole) and 3 parts of a vulcanizing agent S (sulfur).
Mixing: the method comprises the steps of adopting an internal mixer to plasticate three matrix materials of natural rubber, brominated butyl rubber and butadiene rubber together, opening a dust cover and a pressurizing cover of the internal mixer when the temperature of the inner cavity of the internal mixer is increased to 56 ℃, adding stearic acid S.A, dioctyl sebacate DOS, carbon black and zinc oxide ZnO, putting down the dust cover and the pressurizing cover, and opening the dust cover and the pressurizing cover of the internal mixer when the temperature of the internal mixer is increased to 65 ℃ again, wherein Al (OH) is added in two times 3 、Sb 2 O 3 And an anti-aging agent RD, heating to 78 ℃ for discharging, then transferring to an open mill, carrying out sheet feeding in the open mill for 5 times, and airing for 3 hours to obtain the primary mixed film.
Adding a vulcanizing agent: and (3) switching on cooling water of an open mill, locking the roll gap, thinly passing the primary mixed film which is parked at room temperature for 3 hours on the open mill for 3 times, adjusting the roll gap of a double-roll rubber mill to ensure that the rubber material is wrapped by the rolls, keeping a small amount of residual rubber above the two rolls, adding the accelerator M and the vulcanizing agent S, and thinly passing for 8 times to obtain the rubber compound after the accelerator M and the vulcanizing agent S are completely mixed into the rubber.
Preparation of damping Structure
Example 2
Firstly, washing the surface of an aluminum plate for 1 time sequentially by using a cleaning agent, tap water and distilled water, brushing Chemlok205 primer on the aluminum plate after airing, putting the aluminum plate into a gluing cabinet, setting the temperature of the gluing cabinet to be 35+/-5 ℃, standing for 30min, then coating a Chemlok220LF surface adhesive, putting the aluminum plate into the gluing cabinet, setting the temperature of the gluing cabinet to be 35+/-5 ℃, and standing for 40min for later use.
Then, assembling the damping structure with a die (comprising a middle die, an upper die and a lower die), and placing the damping structure on a lower die plate of a vulcanization molding machine, wherein the temperatures of the upper die plate and the lower die plate of the vulcanization molding machine are set to 145 ℃; and closing the die and preheating the die for 45min.
Setting the roller temperature of the four-roller rubber calender to 55 ℃, setting the roller spacing of the four-roller rubber calender to 1.3mm, setting the cutter distance to 600mm, placing the rubber compound on a double-roller rubber mill, back milling until the rubber compound is soft and smooth in surface, placing the back-milled rubber compound at the rubber feeding position of the four-roller rubber calender, enabling the rubber compound to be wrapped into uniform rubber sheets, and testing the thickness of the rubber sheets to 1.3-1.4 mm by using a thickness gauge. And (5) blanking by using a scraper when the surface of the film is leveled, and attaching the mixed film and the isolation cloth to a roller for coiling.
After coiling, the rolled film is sheared into blanks with the side length of 485 mm-492 mm.
Then, starting a vulcanization molding machine, separating an upper die from a middle die, taking out the middle die, laying an aluminum plate coated with an adhesive in a cavity of a lower die, enabling one surface of the aluminum plate with the adhesive to face upwards, installing the middle die on the lower die, removing isolation cloth on a blank, laying the blank on the aluminum plate, closing the die, exhausting for 12 times, starting vulcanization after exhausting is completed, setting the gauge pressure of vulcanization pressure to be 15MPa, and setting the vulcanization time to be 15min.
And after the vulcanization is finished, unloading the mould, taking out the semi-finished product of the damping structure, and removing the redundant sizing material at the edge by using a wallpaper knife.
And (3) placing one surface of the damping structure semi-finished product with the rubber layer upwards into a laminating machine, completely attaching the acrylic pressure-sensitive adhesive on the rubber layer through the laminating machine, and cutting off redundant double-sided adhesive by the laminating machine to obtain the damping structure finished product.
The damping structure prepared in example 2 was subjected to a sound insulation test, a damping loss factor test and a flame retardant property test, and the test results are shown in tables 1 to 5.
The sound insulation amount was measured by referring to the specification of ASTM E2249, and the sound insulation test room was composed ofThe sound source room is a reverberation room, and the receiving room is a semi-silencing room or a full-silencing room. The damping structure is arranged in the wall body between the sound source chamber and the receiving chamber, and the area is not less than 1.0m 2 . And scanning and testing the sound power level in the receiving room by adopting a sound intensity probe. The test results are shown in Table 1.
TABLE 1 Sound insulation test results
As can be seen from table 1, the sound insulation test is performed before and after the typical piece of skin with the specification of 1.2×1.2 is laid down with the damping structure, and the insertion loss at 1000Hz is not less than 1dB. The invention has excellent sound insulation and noise reduction performance.
The damping loss factor was tested with reference to the specifications of ASTM E756, the test results are shown in table 2 below.
Table 2 damping loss factor test results
As can be seen from Table 2, the damping structure is stuck on the base beam for cantilever beam test, and the damping loss factor of the damping structure is not less than 0.3 at 50 Hz-1000 Hz, -40 ℃ to-20 ℃. The invention has excellent damping and vibration-reducing performance at-40 ℃ to-20 ℃.
The flame retardant performance was tested with reference to the regulations of the national aviation regulation CCAR25 section, and the test results are shown in tables 3 to 5 below.
TABLE 3 12s vertical burn test results
TABLE 4 smoke density test results
TABLE 5 flame spread test results
It can be seen from tables 3-5 that the damping structure of the present invention passed the 12s vertical burn, smoke density and burn and flame spread assessment. The damping structure of the invention completely meets the requirement of the navigable standard on flame retardance.
The present invention is not limited to the above-mentioned embodiments, and any changes or substitutions that can be easily understood by those skilled in the art within the technical scope of the present invention are intended to be included in the scope of the present invention. Therefore, the protection scope of the present invention shall be subject to the protection scope of the claims.

Claims (9)

1. The rubber compound for the damping structure is characterized by being mainly prepared from the following raw materials in a mixing manner:
65-75 parts of natural rubber, 15-25 parts of brominated butyl rubber and 5-15 parts of butadiene rubber;
the raw materials also comprise: 65-75 parts of a first flame retardant and 35-45 parts of a second flame retardant, wherein the first flame retardant is aluminum hydroxide, and the second flame retardant is antimony trioxide.
2. The rubber compound according to claim 1, wherein the mass ratio of the natural rubber, the brominated butyl rubber and the butadiene rubber is (6.8-7.2): 1.8-2.2): 0.8-1.2.
3. A rubber compound according to claim 1 or 2, characterized in that the raw materials further comprise: 10-15 parts of reinforcing agent, 1-3 parts of first plasticizer, 8-10 parts of second plasticizer, 3-6 parts of active agent, 1-2 parts of anti-aging agent, 2-3 parts of accelerator and 2-3 parts of vulcanizing agent.
4. A rubber compound according to claim 3, characterized in that,
the reinforcing agent is carbon black;
the first plasticizer is stearic acid;
the second plasticizer is dioctyl sebacate;
the active agent is zinc oxide;
the anti-aging agent comprises one or more of quinoline polymer, imidazole polymer and p-phenylenediamine;
the accelerator comprises one or more of tetramethyl thiuram and benzothiazole;
the vulcanizing agent is sulfur.
5. A rubber layer for a damping structure, characterized in that it is formed from the rubber compound of any one of claims 1-4.
6. The damping structure is characterized by comprising the following components in sequence from bottom to top: a pressure sensitive adhesive layer, the rubber layer of claim 5, and a constraining layer.
7. The damping structure of claim 6, wherein the constraining layer is an aluminum plate; the pressure-sensitive adhesive layer is made of acrylic ester materials.
8. The preparation method of the damping structure is characterized by comprising the following steps of:
forming the rubber compound of any one of claims 1-4 into a film;
preheating a die for forming a damping structure;
providing a constraint layer, and coating an adhesive on the constraint layer;
placing the coated restraint layer and the film in a reserved mould for vulcanization molding;
after vulcanization molding is finished, unloading the mold to take out a damping structure semi-finished product, wherein the damping structure semi-finished product comprises a constraint layer and a rubber layer; and
and forming a pressure-sensitive adhesive layer on the rubber layer to obtain the damping structure.
9. The method of preparing the film according to claim 8, wherein the method of preparing the film comprises the steps of:
mixing all the components for preparing the rubber compound, and thinning the lower piece to obtain the rubber compound;
and (5) wrapping the rubber compound into a film.
CN202211192130.0A 2022-09-28 2022-09-28 Rubber compound, rubber layer, damping structure and preparation method thereof Active CN115521514B (en)

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