CN112457544B - Preparation method of benzoxazine-modified butyl rubber wide-temperature-range damping composite material - Google Patents
Preparation method of benzoxazine-modified butyl rubber wide-temperature-range damping composite material Download PDFInfo
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- CN112457544B CN112457544B CN202011293610.7A CN202011293610A CN112457544B CN 112457544 B CN112457544 B CN 112457544B CN 202011293610 A CN202011293610 A CN 202011293610A CN 112457544 B CN112457544 B CN 112457544B
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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
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- 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
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- C08K2003/2296—Oxides; Hydroxides of metals of zinc
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Abstract
The invention discloses a preparation method of a benzoxazine modified butyl rubber wide-temperature-range damping composite material, which comprises the steps of putting butyl rubber, benzoxazine and sodium hydride into a rheometer to react for a period of time to discharge a rubber material, plasticizing the rubber material on a double-roller open mill, sequentially adding a filler, stearic acid, zinc oxide, TMTD, DM and sulfur to blend uniformly, packaging in a triangular bag, turning over for several times, thinly passing, discharging, standing for 24-48 h to remove bubbles, and preparing raw rubber for later use; and vulcanizing the crude rubber on a flat vulcanizing instrument to obtain the benzoxazine modified butyl rubber composite damping material. The modified butyl rubber is obtained by a solvent-free method, so that the problems of complex operation, high cost and the like are solved, the polar group is introduced, the damping temperature range and the damping factor of the butyl rubber are improved, and the application field of the butyl rubber damping material is widened.
Description
Technical Field
The invention belongs to the field of polymer damping materials, and particularly relates to a preparation method of a butyl rubber-based damping composite material obtained by benzoxazine modified butyl rubber in a sodium hydride system.
Background
At present, about 70 percent of domestic vibration and noise reduction materials for vehicles are asphalt-based damping materials, the sources of the materials are wide, the price of the materials is low, but the damping performance of the damping materials is poor due to low-temperature embrittlement, and the damping effects of the damping materials are lost due to high-temperature aging. In addition, asphalt-based damping materials have environmental protection problems, and the asphalt contains polycyclic aromatic hydrocarbons such as anthracene, phenanthrene and pyrene which are difficult to volatilize, and the substances can generate great harm to human bodies after being contacted with the human bodies for a long time, so that the damping materials for foreign vehicles increasingly adopt synthetic polymers as the base materials of the damping sheets.
The rubber material can generate internal friction by means of the internal friction of a macromolecular chain segment near the glass transition temperature, so that the aim of vibration reduction and noise reduction is effectively fulfilled, and the rubber material becomes a hot door in the research of damping materials. The butyl rubber (IIR) is formed by cation copolymerization of a small amount of isoprene and isobutene, wherein the content of isobutene is about 98%, lateral methyl groups on a molecular chain are very dense, and a worm-shaped structure is formed, so that the butyl rubber has a high loss factor. IIR has a damping performance different from that of a common elastomer due to the fact that secondary transition exists near the glass transition temperature, and the internal consumption peak is high and wide. But the effective damping function area is concentrated in a low-temperature area, almost loses the damping function at the temperature of more than 15 ℃, and cannot meet the requirement of normal working temperature, so that the butyl rubber damping composite material with wide temperature range and high damping is obtained by modifying the butyl rubber damping composite material.
Disclosure of Invention
Aiming at the problems in the prior art, the invention provides a preparation method of a benzoxazine modified butyl rubber wide-temperature-range damping composite material. The method adopts a solvent-free bulk method to graft benzoxazine on the butyl rubber, introduces polar groups, namely benzene rings and double bonds, and improves the damping performance of the butyl rubber. And the method is simple to operate and reduces the cost.
The technical scheme of the invention is as follows:
a preparation method of a benzoxazine modified butyl rubber wide temperature range damping composite material comprises the following steps:
(1) at a certain temperature, adding the butyl rubber IIR and NaH into a Haake torque rheometer to react for 10-20 min, then adding benzoxazine, continuing to react for 10-20 min, stopping the reaction, and discharging the rubber material;
(2) plasticizing a rubber material on a double-roller open mill, sequentially adding filler bentonite, stearic acid, zinc oxide, tetramethyl thiuram TMTD, dibenzothiazyl disulfide DM and sulfur, uniformly blending, then packaging in a triangular bag, turning over for several times, thinly passing, slicing, standing for 24-48 h, and removing bubbles to prepare raw rubber for later use;
(3) and (3) vulcanizing the raw rubber obtained in the step (2) on a flat vulcanizing instrument to obtain the benzoxazine modified butyl rubber composite damping material.
Further, in the step (1), by mass, 100 parts of butyl rubber, 10-50 parts of sodium hydride and 10-50 parts of benzoxazine are used.
Further, in the step (1), the mass ratio of the benzoxazine to the sodium hydride is 1: 1.
further, in the step (2), by mass, 10-30 parts of filler, 2 parts of stearic acid, 5 parts of zinc oxide, 2 parts of TMTD, 1 part of DM and 2 parts of sulfur are added.
Further, in the step (3), the vulcanization temperature is 160-180 ℃, the vulcanization pressure is 10-13 MPa, and the vulcanization time is 20-22 min.
The invention has the beneficial effects that:
(1) the benzoxazine modified butyl rubber wide-temperature-range damping composite material prepared by the invention is widely applied to various vehicles such as automobiles, trains, airplanes and the like and engineering machinery, and is used for reducing the damage of vibration and noise generated in the operation process of various mechanical equipment such as automobiles and the like to the health of machinery and people;
(2) the method adopts a solvent-free method, reduces the separation and purification operations of the polymer and reduces the cost; and a polar group is introduced, so that the damping performance is improved.
(3) Compared with the traditional asphalt-based damping pad, the butyl rubber composite damping material obtained by the invention has more excellent damping performance and more stable performance, the performance is not greatly influenced by the change of temperature, and harmful substances and peculiar smell to human bodies are not generated in the using process;
(4) compared with the common resin blending modified butyl rubber damping, the novel thermosetting resin benzoxazine modified butyl rubber has the advantages of greatly improving the thermal stability, the heat resistance and the wear resistance, and having good compatibility with the butyl rubber.
Drawings
FIG. 1 is a tan delta-T relationship diagram of a damping composite without added filler and benzoxazine;
1.2.3 in FIG. 2 are tan delta-T relationship diagrams of the damping composite material with the filler added but without the benzoxazine, and the filler and the benzoxazine respectively;
FIG. 3 is a graph of tan delta-T relationship for 1.2.3.4.5 damping composite material in an embodiment;
FIG. 4 is a cross-sectional profile of a damping composite without added filler and benzoxazine;
FIG. 5 is a cross-sectional profile of a damping composite with added filler but no benzoxazine;
FIG. 6 is a cross-sectional profile of a damping composite with added fillers and benzoxazine;
FIG. 7 is an infrared spectrum of a damping composite obtained with different additives, wherein 1 is a damping composite without filler and benzoxazine; 2, a damping composite material added with filler and without benzoxazine; 3, the damping composite material is prepared by adding benzoxazine without adding filler; and 4, adding a damping composite material of a filler and benzoxazine.
Detailed Description
The coating comprises, by weight, 100 parts of butyl rubber, 10-50 parts of NaH, 10-50 parts of benzoxazine resin, 10-30 parts of filler, 2 parts of stearic acid, 5 parts of zinc oxide, TMTD2 parts, DM1 parts and 2 parts of sulfur. Plasticizing butyl rubber on a double-roller open mill, adding filler, stearic acid, zinc oxide, TMTD, DM, sulfur and benzoxazine in sequence, blending uniformly, then packaging in a triangular bag, turning over for 7 times, thinly passing, slicing, standing for 24h, removing bubbles, and preparing raw rubber for later use. And vulcanizing on a flat vulcanizing instrument at the vulcanizing temperature of 160-180 ℃, under the vulcanizing pressure of 10-13 MPa, and for 20-22 min to obtain the benzoxazine modified butyl rubber composite damping material.
In order to make the aforementioned objects, features and advantages of the present invention comprehensible, embodiments accompanied with figures are described in detail below. The invention is not limited to the embodiments listed but also comprises any other known variations within the scope of the invention as claimed.
Reference herein to "one embodiment" or "an embodiment" means that a particular feature, structure, or characteristic may be included in at least one implementation of the invention. The appearances of the phrase "in one embodiment" in various places in the specification are not necessarily all referring to the same embodiment, nor are separate or alternative embodiments mutually exclusive of other embodiments.
Example 1
100 parts of butyl rubber, 10 parts of benzoxazine, 10 parts of sodium hydride, 10 parts of filler, 2 parts of stearic acid, 5 parts of zinc oxide, 2 parts of TMTD, 1 part of DM and 2 parts of sulfur. Reacting butyl rubber, benzoxazine and sodium hydride in a rheometer for a certain time, discharging the rubber material, plasticizing the rubber material on a double-roll open mill, sequentially adding filler, stearic acid, zinc oxide, TMTD, DM and sulfur, uniformly blending, packaging in a triangular bag, turning over for 7 times, thinly passing, slicing, standing for 24 hours, and removing bubbles to obtain raw rubber for later use. And vulcanizing on a flat vulcanizing instrument at the vulcanizing temperature of 170 ℃, the vulcanizing pressure of 10MPa and the vulcanizing time of 22min to obtain the benzoxazine modified butyl rubber composite damping material.
The modified butyl rubber prepared in example 1 has a high temperature damping temperature range of 60 ℃ or higher and a damping factor of 0.31 at 60 ℃, as shown in curve 1 of FIG. 3.
Example 2
100 parts of butyl rubber, 20 parts of benzoxazine, 20 parts of sodium hydride, 10 parts of filler, 2 parts of stearic acid, 5 parts of zinc oxide, 2 parts of TMTD, 1 part of DM and 2 parts of sulfur. Reacting butyl rubber, benzoxazine and sodium hydride in a rheometer for a certain time, discharging the rubber material, plasticizing the rubber material on a double-roll open mill, sequentially adding filler, stearic acid, zinc oxide, TMTD, DM and sulfur, uniformly blending, packaging in a triangular bag, turning over for 7 times, thinly passing, slicing, standing for 24 hours, and removing bubbles to obtain raw rubber for later use. And vulcanizing on a flat vulcanizing instrument at the vulcanizing temperature of 165 ℃, the vulcanizing pressure of 11MPa and the vulcanizing time of 22min to obtain the benzoxazine modified butyl rubber composite damping material.
The modified butyl rubber prepared in example 2 has a high temperature damping temperature range of 60 ℃ or more and a damping factor of 0.31 at 60 ℃, as shown in curve 2 of FIG. 3.
Example 3
100 parts of butyl rubber, 30 parts of benzoxazine, 30 parts of sodium hydride, 10 parts of filler, 2 parts of stearic acid, 5 parts of zinc oxide, 2 parts of TMTD, 1 part of DM and 2 parts of sulfur. Reacting butyl rubber, benzoxazine and sodium hydride in a rheometer for a certain time, discharging the rubber material, plasticizing the rubber material on a double-roll open mill, sequentially adding filler, stearic acid, zinc oxide, TMTD, DM and sulfur, uniformly blending, packaging in a triangular bag, turning over for 7 times, thinly passing, slicing, standing for 24 hours, and removing bubbles to obtain raw rubber for later use. And vulcanizing on a flat vulcanizing instrument at the vulcanizing temperature of 165 ℃, the vulcanizing pressure of 12MPa and the vulcanizing time of 21min to obtain the benzoxazine modified butyl rubber composite damping material.
The modified butyl rubber prepared in example 3 has a high temperature damping temperature range of 60 ℃ or higher and a damping factor of 0.38 at 60 ℃, as shown in curve 3 of FIG. 3.
Example 4
100 parts of butyl rubber, 40 parts of benzoxazine, 40 parts of sodium hydride, 10 parts of filler, 2 parts of stearic acid, 5 parts of zinc oxide, 2 parts of TMTD, 1 part of DM and 2 parts of sulfur. Reacting butyl rubber, benzoxazine and sodium hydride in a rheometer for a certain time, discharging the rubber material, plasticizing the rubber material on a double-roll open mill, sequentially adding filler, stearic acid, zinc oxide, TMTD, DM and sulfur, uniformly blending, packaging in a triangular bag, turning over for 7 times, thinly passing, slicing, standing for 24 hours, and removing bubbles to obtain raw rubber for later use. And vulcanizing on a flat vulcanizing instrument at the vulcanizing temperature of 170 ℃, the vulcanizing pressure of 12MPa and the vulcanizing time of 20min to obtain the benzoxazine modified butyl rubber composite damping material.
The modified butyl rubber prepared in example 4 has a high temperature damping temperature range of 60 ℃ or higher and a damping factor of 0.34 at 60 ℃, as shown in curve 4 of FIG. 3.
Example 5
100 parts of butyl rubber, 50 parts of benzoxazine, 50 parts of sodium hydride, 10 parts of filler bentonite, 2 parts of stearic acid, 5 parts of zinc oxide, 2 parts of TMTD, 1 part of DM and 2 parts of sulfur. Reacting butyl rubber, benzoxazine and sodium hydride in a rheometer for a certain time, discharging the rubber material, plasticizing the rubber material on a double-roll open mill, sequentially adding filler, stearic acid, zinc oxide, TMTD, DM and sulfur, uniformly blending, packaging in a triangular bag, turning over for 7 times, thinly passing, slicing, standing for 24 hours, and removing bubbles to obtain raw rubber for later use. And vulcanizing on a flat vulcanizing instrument at the vulcanizing temperature of 165 ℃, the vulcanizing pressure of 12MPa and the vulcanizing time of 22min to obtain the benzoxazine modified butyl rubber composite damping material.
The modified butyl rubber prepared in example 5 has a high temperature damping temperature range of 60 ℃ or higher and a damping factor of 0.32 at 60 ℃, as shown in curve 5 of FIG. 3.
Example 6
100 parts of butyl rubber, 10 parts of benzoxazine, 10 parts of sodium hydride, 20 parts of filler bentonite, 2 parts of stearic acid, 5 parts of zinc oxide, 2 parts of TMTD, 1 part of DM and 2 parts of sulfur. Reacting butyl rubber, benzoxazine and sodium hydride in a rheometer for a certain time, discharging the rubber material, plasticizing the rubber material on a double-roll open mill, sequentially adding filler, stearic acid, zinc oxide, TMTD, DM and sulfur, uniformly blending, packaging in a triangular bag, turning over for 7 times, thinly passing, slicing, standing for 24 hours, and removing bubbles to obtain raw rubber for later use. And vulcanizing on a flat vulcanizing instrument at the vulcanizing temperature of 170 ℃, the vulcanizing pressure of 12MPa and the vulcanizing time of 21min to obtain the benzoxazine modified butyl rubber composite damping material.
The modified butyl rubber prepared in example 6 has a high temperature damping temperature range of 42.1 ℃ or more and a damping factor of 0.32 at 42 ℃.
Example 7
100 parts of butyl rubber, 10 parts of benzoxazine, 10 parts of sodium cyanide, 30 parts of filler, 2 parts of stearic acid, 5 parts of zinc oxide, 2 parts of TMTD, 1 part of DM and 2 parts of sulfur. Reacting butyl rubber, benzoxazine and sodium hydride in a rheometer for a certain time, discharging the rubber material, plasticizing the rubber material on a double-roll open mill, sequentially adding filler, stearic acid, zinc oxide, TMTD, DM and sulfur, uniformly blending, packaging in a triangular bag, turning over for 7 times, thinly passing, slicing, standing for 24 hours, and removing bubbles to obtain raw rubber for later use. And vulcanizing on a flat vulcanizing instrument at the vulcanizing temperature of 170 ℃, the vulcanizing pressure of 10MPa and the vulcanizing time of 22min to obtain the benzoxazine modified butyl rubber composite damping material.
The modified butyl rubber prepared in example 7 has a high temperature damping temperature range of 45.3 ℃ or more and a damping factor of 0.35 at 45 ℃.
Example 8
100 parts of butyl rubber, 10 parts of sodium cyanide, 20 parts of filler, 2 parts of stearic acid, 5 parts of zinc oxide, 2 parts of TMTD, 1 part of DM and 2 parts of sulfur. Reacting butyl rubber and sodium hydride in a rheometer for a certain time, discharging the rubber material, plasticizing the rubber material on a double-roll open mill, sequentially adding filler, stearic acid, zinc oxide, TMTD, DM and sulfur, uniformly blending, packaging in a triangular bag, turning over for 7 times, thinly passing, slicing, standing for 24 hours, and removing bubbles to obtain raw rubber for later use. And vulcanizing on a flat vulcanizing instrument at the vulcanizing temperature of 180 ℃, under the vulcanizing pressure of 12MPa and for 22min to obtain the benzoxazine modified butyl rubber composite damping material.
The high-temperature damping temperature range of the modified butyl rubber prepared in the embodiment 8 is less than or equal to 45.8 ℃, and the damping factor at 45 ℃ is 0.30.
Comparing the high-damping wide-temperature-range butyl rubber damping composite material for vehicles prepared by the methods of examples 1-5 of the present invention with the damping composite material without modified resin and/or filler, please refer to fig. 1-7 and table 1 for specific properties
TABLE 1
As seen from Table 1, the tensile strength and tear strength of the damping composite material obtained by adding the benzoxazine resin are increased.
From fig. 3, it can be seen that the maximum damping factor of the damping composite material obtained by adding the thermosetting resin benzoxazine is reduced, but the effective damping temperature range (the temperature range of the damping factor is more than or equal to 0.3) of the damping composite material is widened, wherein the damping temperature range of the damping composite material obtained by adding the benzoxazine and the filler extends to more than 65 ℃, and the industrial requirement is met;
it can be seen from fig. 2 that the damping temperature range of the damping composite material is improved by the addition of the filler, but the tensile strength and the tear strength are slightly reduced, because the added filler is a non-reinforced filler, when the molecular chain moves, the loss is increased by the friction between the filler and the matrix, and the filler, so that a wider damping temperature range is shown, but a certain bonding glue is formed on the surface of the filler, so that the proportion of the raw glue is reduced, and the maximum damping factor is reduced, while the bonding effect between the non-reinforced filler and the matrix is not strong, and because of stress concentration and orientation, the tensile strength, the tear strength and the like of the obtained damping composite material are slightly reduced, but the service performance is not influenced.
As can be seen from fig. 4, 5 and 6, the SEM images of pure butyl rubber have a smoother cross-section and the cross-section becomes rough after the addition of bentonite. With the addition of the filler and the benzoxazine together, molecular chains are attached to the surface of the filler through adsorption and winding to form bonding glue, so that the friction opportunities among the molecular chains of the butyl rubber, the filler, the molecular chains, the benzoxazine and the filler and the benzoxazine are increased, the molecular chains are difficult to move, and the internal consumption is increased.
It can be seen from fig. 7, curves 1 and 2 that the infrared spectrograms of vulcanized pure butyl rubber damping material and added kaolin are analyzed by comparison, and it is found that the positions of absorption peaks in a spectrogram of pure butyl rubber are not changed after the filler is added, and new absorption peaks are not formed due to chemical reaction and the like. Comparing curves 1, 3 and 4, it can be known that the functional group in benzoxazine increases friction with butyl rubber molecular chain and filler, and increases internal friction.
In conclusion, the preparation method of the benzoxazine modified butyl rubber wide-temperature-range damping composite material is simple in operation method; the heat stability, heat resistance and wear resistance of the product are greatly improved, and the damage of vibration and noise generated in the running process of various mechanical equipment such as automobiles to the health of machinery and people can be reduced.
It should be noted that the above-mentioned embodiments are only for illustrating the technical solutions of the present invention and not for limiting, and although the present invention has been described in detail with reference to the preferred embodiments, it should be understood by those skilled in the art that modifications or equivalent substitutions may be made on the technical solutions of the present invention without departing from the spirit and scope of the technical solutions of the present invention, which should be covered by the claims of the present invention.
Claims (5)
1. A preparation method of a benzoxazine modified butyl rubber wide temperature range damping composite material is characterized by comprising the following steps:
(1) adding the butyl rubber IIR and NaH into a Haake torque rheometer to react for 10-20 min, then adding benzoxazine, continuing to react for 10-20 min, stopping the reaction, and discharging the rubber material;
the rubber comprises, by mass, 100 parts of butyl rubber, 10-50 parts of sodium hydride and 10-50 parts of benzoxazine;
(2) plasticizing rubber materials on a double-roller open mill, sequentially adding filler bentonite, stearic acid, zinc oxide, tetramethyl thiuram TMTD, dibenzothiazyl disulfide DM and sulfur, uniformly blending, then packaging in a triangular bag, turning over for several times, thinly passing, discharging, standing and removing bubbles to prepare raw rubber for later use;
(3) and (3) vulcanizing the raw rubber obtained in the step (2) on a flat vulcanizing instrument to obtain the benzoxazine modified butyl rubber wide-temperature-range damping composite material.
2. The method of claim 1, wherein: the mass ratio of the benzoxazine to the sodium hydride is 1: 1.
3. the method of claim 1, wherein: in the step (2), by mass, 10-30 parts of filler, 2 parts of stearic acid, 5 parts of zinc oxide, 2 parts of TMTD, 1 part of DM and 2 parts of sulfur are used.
4. The method of claim 1, wherein: in the step (2), the time for removing bubbles is 24-48 h.
5. The method of claim 1, wherein: in the step (3), the vulcanization temperature is 160-180 ℃, the vulcanization pressure is 10-12 MPa, and the vulcanization time is 20-22 min.
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| CN113480201B (en) * | 2021-08-24 | 2022-10-14 | 揭阳市东信智能门窗科技有限公司 | Anti-noise hollow glass and preparation method thereof |
| CN115960419A (en) * | 2022-12-27 | 2023-04-14 | 安徽顺豪新材料科技有限公司 | Preparation process of high-thermal-stability automobile damping film |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1179442A (en) * | 1996-10-07 | 1998-04-22 | 拜尔公司 | Polymer compounds and their use for vulcanisation of halogenated butyl rubbers with low halogen content |
| CN110437550A (en) * | 2019-08-05 | 2019-11-12 | 常州浩达科技股份有限公司 | The preparation method of the automobile-used wide temperature range butyl rubber damp composite material of high-damping |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1179442A (en) * | 1996-10-07 | 1998-04-22 | 拜尔公司 | Polymer compounds and their use for vulcanisation of halogenated butyl rubbers with low halogen content |
| CN110437550A (en) * | 2019-08-05 | 2019-11-12 | 常州浩达科技股份有限公司 | The preparation method of the automobile-used wide temperature range butyl rubber damp composite material of high-damping |
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