CN111423655B - Environment-friendly flame-retardant hot-melt type damping film for automobile and preparation method thereof - Google Patents
Environment-friendly flame-retardant hot-melt type damping film for automobile and preparation method thereof Download PDFInfo
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Abstract
The invention belongs to the technical field of rubber, and particularly relates to an environment-friendly flame-retardant hot-melt type damping film for an automobile and a preparation method thereof. The damping film is prepared from the following raw materials in parts by weight: 35 parts of ethylene-octene copolymer (POE), 30 parts of Ethylene Propylene Diene Monomer (EPDM), 20 parts of ethylene-vinyl acetate copolymer (EVA), 15 parts of Polyethylene (PE), 60-100 parts of barite powder, 60-100 parts of heavy calcium carbonate, 15-30 parts of aluminum hydroxide, 5-20 parts of carbon black, 5 parts of VOC masking agent, 3-4 parts of white oil, 1-3 parts of anti-aging agent and 0.5-1.5 parts of stearic acid. The damping film prepared by the formula of the invention is not only environment-friendly, but also has good flame retardance, can effectively prevent the spread of fire when an automobile fires, is beneficial to escape, and reduces property loss and casualties.
Description
Technical Field
The invention belongs to the technical field of rubber, and particularly relates to an environment-friendly flame-retardant hot-melt type damping film for an automobile and a preparation method thereof.
Background
The damping film is an organic polymer material with viscoelasticity, which is adhered to the inner surface of the automobile body, and the vibration mechanical energy of sound waves is converted into heat energy to be dissipated by utilizing the viscoelasticity of the organic polymer material, so that the purposes of reducing amplitude, reducing vibration and inhibiting noise are achieved, and the damping film has a damping effect.
The existing damping material generates a great amount of smoke during combustion, releases toxic gas, is unfavorable for escape of personnel in a vehicle during fire, and also can pollute the environment. Therefore, there is a need to develop a damping film which is environmentally friendly and has good flame retardant properties.
Disclosure of Invention
The invention aims to provide an environment-friendly flame-retardant hot-melt damping film for an automobile and a preparation method thereof.
Based on the above purpose, the invention adopts the following technical scheme: an environment-friendly flame-retardant hot-melt damping film for automobiles is prepared from the following raw materials in parts by weight:
ethylene-octene copolymer (POE): 35 parts;
ethylene Propylene Diene Monomer (EPDM): 30 parts;
ethylene-vinyl acetate copolymer (EVA): 20 parts;
polyethylene (PE): 15 parts;
barite powder: 60-100 parts;
heavy calcium: 60-100 parts;
aluminum hydroxide: 15-30 parts;
carbon black: 5-20 parts;
VOC masking agents: 5 parts;
white oil: 3-4 parts;
anti-aging agent: 1-3 parts;
stearic acid: 0.5 to 1.5 portions.
Preferably, the hot-melt type damping film is prepared from the following raw materials in parts by weight: 35 parts of POE, 30 parts of EPDM, 20 parts of EVA, 15 parts of PE, 90 parts of barite powder, 60 parts of heavy calcium, 15 parts of aluminum hydroxide, 5 parts of carbon black, 5 parts of VOC masking agent, 4 parts of white oil, 2 parts of anti-aging agent and 1 part of stearic acid.
Preferably, the antioxidant is formed by mixing the antioxidant 1010 and the antioxidant 168 according to a mass ratio of 1:1.
The preparation process of the hot melt type damping film comprises the following steps: the raw materials are put into an internal mixer, evenly mixed at 170 ℃, evenly fed into an extruder, extruded into a three-roll calender through a die at 200 ℃ and pressed into a sheet shape, thus the hot-melt damping film is prepared.
Compared with the prior art, the invention has the beneficial effects that:
the damping film formula with environmental protection performance meeting the technical requirements of car interior parts and material emission performance and flame retardant performance meeting the enterprise standard of Shanghai automobile group Co-Ltd is screened out by adjusting the dosage of auxiliary materials including barite powder, heavy calcium and aluminum hydroxide based on main materials POE, EPDM, EVA and PE. The damping film prepared by the formula of the invention is not only environment-friendly, but also has good flame retardance, can effectively prevent the spread of fire when an automobile fires, is beneficial to escape, and reduces property loss and casualties.
Drawings
FIG. 1 is a graph showing the comparison of the sample 8 before and after combustion in the combustion experiment.
Detailed Description
EXAMPLE 1 Effect of different raw Material Components on damping film Performance
(1) Sample preparation
The amounts of POE, EPDM, EVA, PE, carbon black, VOC masking agent, white oil, antioxidant 1010, antioxidant 168 and stearic acid in the raw materials are kept consistent, and are respectively: 35 parts by weight of POE, 30 parts by weight of EPDM, 20 parts by weight of EVA, 15 parts by weight of PE, 5 parts by weight of carbon black, 5 parts by weight of VOC masking agent, 4 parts by weight of white oil, 1 part by weight of antioxidant 1010, 1 part by weight of antioxidant 168 and 1 part by weight of stearic acid. The different amounts of heavy calcium, barite powder and aluminum hydroxide in the raw materials are regulated, and are shown in table 1.
The raw materials are placed in an internal mixer, evenly mixed at 170 ℃, evenly fed into an extruder, extruded into a three-roll calender at 200 ℃ by a die and pressed into a sheet shape, so that nine different damping films are prepared, wherein the damping films are respectively marked as samples 1-9, the weight parts of heavy calcium, heavy crystal powder and aluminum hydroxide in the samples 1-9 are respectively shown in table 1, meanwhile, the mechanical properties and flame retardant properties of the samples 1-9 are detected, and the detection results are attached to table 1, wherein the flame retardant property test evaluation criteria are shown in table 2.
TABLE 2 horizontal burn Rate evaluation criteria (selected from the group consisting of SMTC 5 400 008-2015)
(2) Performance detection
1) Analysis of mechanical Properties
According to national standard GB/T528-2009, the tensile strength and elongation at break index of samples 1-9 are detected, the detection results are shown in table 1, and it is generally considered that the higher the tensile strength and elongation at break of the damping film, the better the ageing performance, and the longer the service time of the damping film. Although the tensile strength and elongation at break of the prepared damping film tend to decrease with the increase of the dosage of heavy calcium carbonate, barite powder and aluminum hydroxide in the formula, the samples 1 to 9 all meet and are far higher than the chemical industry standard by referring to the specification that the tensile strength of the hot-melt damping film is more than or equal to 0.6Mpa in the chemical industry standard (HG/T4384-2012) of the damping film for automobiles.
2) Analysis of flame retardant Properties
The combustion characteristics of samples 1 to 9 are detected according to the Shanghai automobile group company technology center enterprise standard (SMTC 5 400 008-2015), the detection indexes are the horizontal combustion rate of the samples, the detection results are shown in table 1, wherein the evaluation criteria of the horizontal combustion rate are shown in table 2, and if the combustion speed is less than 100mm/min in the whole measurement section, the result is BR.. If the burning distance is more than 50mm and the burning speed is less than 100mm/min, the result is recorded as SE/BR.. If the burning distance is not more than 50mm and the burning time is less than 60s, the fuel is SE/NBR; the results of the combustion characteristics not conforming to table 2 are recorded as easy combustion.
As can be seen from the results in table 1, when no heavy calcium, heavy crystal powder and aluminum hydroxide are added to the raw materials, the prepared damping film sample (sample 1) is flammable and does not meet the enterprise standard; samples 2, 3, 4 and 9 are prepared from one or two auxiliary materials of heavy calcium, barite powder and aluminum hydroxide, the burning speed of the prepared damping film samples 2, 3, 4 and 9 is greater than 50mm/min and less than 100mm/min, and the burning grade is SE/BR grade; samples 5, 6, 7 and 8, namely triple superphosphate, barite powder and aluminum hydroxide are mixed for use, the burning speed of the prepared damping film sample is less than 50mm/min, the flame retardant performance grade is SE/NBR, and the flame retardant grade is highest. Namely, compared with a damping film prepared from any one or two of triple superphosphate, barite powder and aluminum hydroxide, the damping film prepared from the triple superphosphate, the barite powder and the aluminum hydroxide has better flame retardant property when the triple superphosphate, the barite powder and the aluminum hydroxide are combined.
Further analysis of the raw material composition, mechanical properties and flame retardant properties of samples 5 to 8 shows that the tensile strength and elongation at break of sample 8 are slightly better than those of samples 5 to 7 under the condition that the flame retardant properties of samples 5 to 8 are close; in addition, as can be deduced from comparison of the combustion performance of samples 2, 3 and 9, the addition of aluminum hydroxide can improve the flame retardant performance of the damping film relative to the heavy calcium and the barite powder. However, in the actual processing process, as the usage amount of aluminum hydroxide increases, the hardness of the rubber material increases, the fluidity becomes poor, and the processing performance is reduced, so that the damping rubber sheet can be prepared at a higher mixing temperature and extrusion temperature, and the processing cost of the damping rubber sheet is increased. Therefore, the preparation formula of the sample 8 is taken as the optimal formula by comprehensively considering the mechanical property, the processing property and the cost of the damping film.
(3) Taking sample 8 as an example, the aging performance, the environmental protection performance and the flame retardance of the damping film of the invention are further detected and analyzed
1) Aging Properties
Because the damping film generates aging phenomenon along with time in the use process, the film becomes hard and brittle, and the service performances such as damping are lost, the aging performance of the damping film is necessary to be detected. Taking a damping film of the sample 8 as an example, carrying out Shore A hardness detection on the sample 8 according to national standard GB/T531-2009; according to national standard GB/T528-2009, the tensile strength and elongation at break of the sample 8 are detected. And then aging the damping film at 120 ℃ for 720 hours, cooling to room temperature, and detecting the properties of Shore A hardness, tensile strength and breaking elongation of the damping film again.
And (3) additionally taking the damping film of the sample 8, treating the damping film at 200 ℃ for 3min, cooling to room temperature, namely pre-shrinking the damping film, then storing the pre-shrunk film at 90 ℃ for 24h, cooling to room temperature, and detecting the shrinkage rate of the film after treatment.
As shown in Table 3, the Shore A hardness of the damping film of sample 8 is increased by 7, the transverse tensile strength is reduced by 11.7%, the longitudinal tensile strength is reduced by 13.3%, the transverse elongation at break is reduced by 11.9%, and the longitudinal elongation at break is reduced by 15.1%, although the tensile strength and elongation at break of the damping film after aging are reduced, the reduction is small, and the damping film after aging still meets the specification that the tensile strength of the hot-melt damping film is more than or equal to 0.6Mpa in industry standard (HG/T4384-2012).
The shrinkage rate of the damping film after shrinkage treatment is 1.23 percent, and meets the specification that the shrinkage rate of the damping film is less than or equal to 2 percent in the chemical industry standard (HG/T4384-2012) of the damping film for automobiles.
In conclusion, the aging performance of the damping film prepared by the formula disclosed by the invention meets the industry standard, and the damping film has the service life specified by the industry standard.
2) Environmental protection performance
Sample 8 was subjected to environmentally friendly detection of Volatile Organic Compounds (VOCs) according to the detection method specified in SMTC 5 400 018-2019, and the detection results are shown in Table 4. As can be seen from the detection results in Table 4, each detection item of VOC in the damping film is qualified, and meets the specification of the technical requirements (SMTC 5 300 004-2015 (V3)) for the emission performance of interior parts and materials of cars.
3) Flame retardant Properties
The combustion characteristic of the damping film of the sample 8 is detected according to the technical center enterprise standard (SMTC 5 400 008-2015) of Shanghai automobile group Co., ltd. The detection result is shown in figure 1, figure 1 is a comparison chart of 5 parallel samples of the damping film of the sample 8 before and after combustion, and as can be seen from figure 1, the sample 8 is detected according to the SMTC 5 400 008-2015 standard, the combustion distance is less than 50mm, the combustion time is less than 60s, and the damping film is a self-extinguishing sample with highest flame retardant level.
In summary, the environmental protection performance of the damping film prepared according to the formula of the invention meets the specification of the technical requirements of the automotive interior parts and the material emission performance, and the flame retardant performance of the damping film meets the enterprise standard of Shanghai automobile group Co-Ltd; the damping film prepared by the formula of the invention is not only green and environment-friendly, but also has good flame retardance.
Example 2
An environment-friendly flame-retardant hot-melt damping film for automobiles is prepared from the following raw materials in parts by weight: 35 parts of POE, 30 parts of EPDM, 20 parts of EVA, 15 parts of PE, 60 parts of barite powder, 100 parts of heavy calcium carbonate, 15 parts of aluminum hydroxide, 20 parts of carbon black, 5 parts of VOC masking agent, 3 parts of white oil, 1.5 parts of antioxidant 1010, 1.5 parts of antioxidant 168 and 0.5 part of stearic acid.
The raw materials are put into an internal mixer, evenly mixed at 170 ℃, evenly fed into an extruder, extruded into a three-roll calender through a die at 200 ℃ and pressed into a sheet shape, thus the hot-melt damping film is prepared.
Example 3
An environment-friendly flame-retardant hot-melt damping film for automobiles is prepared from the following raw materials in parts by weight: 35 parts of POE, 30 parts of EPDM, 20 parts of EVA, 15 parts of PE, 100 parts of barite powder, 60 parts of heavy calcium carbonate, 30 parts of aluminum hydroxide, 5 parts of carbon black, 5 parts of VOC masking agent, 4 parts of white oil, 0.5 part of antioxidant 1010, 0.5 part of antioxidant 168 and 1.5 parts of stearic acid.
The raw materials are put into an internal mixer, evenly mixed at 170 ℃, evenly fed into an extruder, extruded into a three-roll calender through a die at 200 ℃ and pressed into a sheet shape, thus the hot-melt damping film is prepared.
Example 4
An environment-friendly flame-retardant hot-melt damping film for automobiles is prepared from the following raw materials in parts by weight: 35 parts of POE, 30 parts of EPDM, 20 parts of EVA, 15 parts of PE, 60 parts of barite powder, 60 parts of heavy calcium carbonate, 15 parts of aluminum hydroxide, 5 parts of carbon black, 5 parts of VOC masking agent, 3 parts of white oil, 0.5 part of antioxidant 1010, 0.5 part of antioxidant 168 and 0.5 part of stearic acid.
The raw materials are put into an internal mixer, evenly mixed at 170 ℃, evenly fed into an extruder, extruded into a three-roll calender through a die at 200 ℃ and pressed into a sheet shape, thus the hot-melt damping film is prepared.
Example 5
An environment-friendly flame-retardant hot-melt damping film for automobiles is prepared from the following raw materials in parts by weight: 35 parts of POE, 30 parts of EPDM, 20 parts of EVA, 15 parts of PE, 100 parts of barite powder, 100 parts of heavy calcium carbonate, 30 parts of aluminum hydroxide, 20 parts of carbon black, 5 parts of VOC masking agent, 4 parts of white oil, 1.5 parts of antioxidant 1010, 1.5 parts of antioxidant 168 and 1.5 parts of stearic acid.
The raw materials are put into an internal mixer, evenly mixed at 170 ℃, evenly fed into an extruder, extruded into a three-roll calender through a die at 200 ℃ and pressed into a sheet shape, thus the hot-melt damping film is prepared.
Example 6
An environment-friendly flame-retardant hot-melt damping film for automobiles is prepared from the following raw materials in parts by weight: 35 parts of POE, 30 parts of EPDM, 20 parts of EVA, 15 parts of PE, 90 parts of barite powder, 80 parts of heavy calcium carbonate, 20 parts of aluminum hydroxide, 10 parts of carbon black, 5 parts of VOC masking agent, 4 parts of white oil, 1 part of antioxidant 1010, 1 part of antioxidant 168 and 1 part of stearic acid.
The raw materials are put into an internal mixer, evenly mixed at 170 ℃, evenly fed into an extruder, extruded into a three-roll calender through a die at 200 ℃ and pressed into a sheet shape, thus the hot-melt damping film is prepared.
Example 7
An environment-friendly flame-retardant hot-melt damping film for automobiles is prepared from the following raw materials in parts by weight: 35 parts of POE, 30 parts of EPDM, 20 parts of EVA, 15 parts of PE, 70 parts of barite powder, 90 parts of heavy calcium carbonate, 25 parts of aluminum hydroxide, 15 parts of carbon black, 5 parts of VOC masking agent, 3 parts of white oil, 1.2 parts of antioxidant 1010, 1.2 parts of antioxidant 168 and 1.5 parts of stearic acid.
The raw materials are put into an internal mixer, evenly mixed at 170 ℃, evenly fed into an extruder, extruded into a three-roll calender through a die at 200 ℃ and pressed into a sheet shape, thus the hot-melt damping film is prepared.
Example 8
An environment-friendly flame-retardant hot-melt damping film for automobiles is prepared from the following raw materials in parts by weight: 35 parts of POE, 30 parts of EPDM, 20 parts of EVA, 15 parts of PE, 80 parts of barite powder, 70 parts of heavy calcium, 15 parts of aluminum hydroxide, 10 parts of carbon black, 5 parts of VOC masking agent, 4 parts of white oil, 1 part of antioxidant 1010, 1 part of antioxidant 168 and 0.5 part of stearic acid.
The raw materials are put into an internal mixer, evenly mixed at 170 ℃, evenly fed into an extruder, extruded into a three-roll calender through a die at 200 ℃ and pressed into a sheet shape, thus the hot-melt damping film is prepared.
Claims (2)
1. The environment-friendly flame-retardant hot-melt type damping film for the automobile is characterized by being prepared from the following raw materials in parts by weight: 35 parts of POE, 30 parts of EPDM, 20 parts of EVA, 15 parts of PE, 90 parts of barite powder, 60 parts of heavy calcium, 15 parts of aluminum hydroxide, 5 parts of carbon black, 5 parts of VOC masking agent, 4 parts of white oil, 2 parts of anti-aging agent and 1 part of stearic acid;
the preparation method of the hot-melt type damping film is characterized by comprising the following steps of: the raw materials are put into an internal mixer, evenly mixed at 170 ℃, evenly fed into an extruder, extruded into a three-roll calender through a die at 200 ℃ and pressed into a sheet shape, so that the hot-melt damping film is prepared.
2. The hot melt type damping film according to claim 1, wherein the anti-aging agent is formed by mixing an antioxidant 1010 and an antioxidant 168 in a mass ratio of 1:1.
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| CN105924805A (en) * | 2016-05-24 | 2016-09-07 | 中山市绿浪助剂有限公司 | Novel insulated rubber cable sheath formula |
| CN106243469A (en) * | 2016-07-29 | 2016-12-21 | 扬州华声电子实业有限公司 | A kind of POE/EPDM component-type environment friendly non-halogen insulation compound and preparation method thereof |
| CN106750860A (en) * | 2016-12-12 | 2017-05-31 | 天长市康宁塑胶科技有限公司 | A kind of high temperature resistant halogen-free flame-retardant thermoplastic elastomer (TPE) and preparation method thereof |
| CN106519643A (en) * | 2016-12-29 | 2017-03-22 | 安徽浩丰特种电子材料有限公司 | High-strength heat-resistant corrosion-resistant polyurethane board and preparation method thereof |
| CN110862603A (en) * | 2019-11-29 | 2020-03-06 | 上海华谷车业有限公司 | Automobile sound insulation pad skin and preparation thereof |
| CN110922688A (en) * | 2019-12-10 | 2020-03-27 | 上海新安汽车隔音毡有限公司 | Manufacturing method of flame-retardant damping cushion for automobile |
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