CN115678281B - Anti-fatigue damping vulcanized rubber and preparation method thereof - Google Patents

Anti-fatigue damping vulcanized rubber and preparation method thereof Download PDF

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Publication number
CN115678281B
CN115678281B CN202211441754.1A CN202211441754A CN115678281B CN 115678281 B CN115678281 B CN 115678281B CN 202211441754 A CN202211441754 A CN 202211441754A CN 115678281 B CN115678281 B CN 115678281B
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parts
damping
rubber
fatigue
carbon black
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CN115678281A (en
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孟思益
刘永亮
陈珏
吴珊
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Aerospace Science and Industry Changsha New Materials Research Institute Co Ltd
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Aerospace Science and Industry Changsha New Materials Research Institute Co Ltd
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Abstract

The invention relates to an anti-fatigue damping vulcanized rubber and a preparation method thereof, which are characterized in that trans-1, 4-polyisoprene rubber and chlorinated butyl rubber are introduced into a phenyl silicone rubber system in a damping filler master batch mode, so that the fatigue resistance of the material can be greatly improved, the prepared vulcanized rubber material has good mechanical property, fatigue resistance and damping property, the problem that the damping material in the prior art cannot meet the multiple requirements of the damping material on damping property, mechanical property and fatigue resistance in the aerospace field is solved, and the obtained rubber material has wide application prospect in the aerospace field.

Description

Anti-fatigue damping vulcanized rubber and preparation method thereof
Technical Field
The invention relates to the technical field of rubber materials, in particular to an anti-fatigue damping vulcanized rubber and a preparation method thereof.
Background
The aircraft can generate vibration during flight, and the vibration frequency of the aircraft ranges from a few hertz to hundreds of hertz. Vibration not only gives people uncomfortable feeling, but also can cause component failure, and strong vibration can cause serious accidents caused by serious damage to the whole aircraft, so that vibration prevention treatment is necessary.
Damping rubber is commonly used as a shock absorber in the current anti-vibration measures in the aerospace field. A good damping rubber shock absorber is required to have high vibration isolation effect, and meanwhile, the performance of the good damping rubber shock absorber is required to keep structural integrity after long-term storage and use, and the performance of the good damping rubber shock absorber is required to be stable. The existing damping material can not meet multiple requirements of the aerospace field on damping performance, mechanical performance and fatigue resistance of the damping material.
Disclosure of Invention
Aiming at the problem that damping performance, mechanical performance and fatigue resistance are difficult to consider in the prior art, one aspect of the invention provides anti-fatigue damping vulcanized rubber, which comprises the following components in parts by weight:
80-120 parts of phenyl silicone rubber;
10-30 parts of damping filler masterbatch;
10-40 parts of white carbon black;
1-4 parts of plasticizer;
1-2 parts of vulcanizing agent;
the damping filler masterbatch comprises the following components in parts by weight:
60-100 parts of chlorinated butyl rubber;
10-50 parts of trans-1, 4-polyisoprene rubber;
20-50 parts of white carbon black;
2-5 parts of plasticizer;
1-4 parts of zinc oxide;
1-3 parts of stearic acid;
0.5-2 parts of sulfur;
0.5 to 2 portions of accelerator.
According to the anti-fatigue damping vulcanized rubber provided by the invention, preferably, the anti-fatigue damping vulcanized rubber comprises the following components in parts by weight: 80-100 parts of phenyl silicone rubber and 15-25 parts of damping filler masterbatch.
According to the anti-fatigue damping vulcanized rubber provided by the invention, preferably, the anti-fatigue damping vulcanized rubber comprises the following components in parts by weight: 30-40 parts of white carbon black.
According to the anti-fatigue damping vulcanized rubber provided by the invention, preferably, the phenyl silicone rubber contains 10-30 mol% of phenyl and 0.05-0.3 mol% of vinyl.
According to the anti-fatigue damping vulcanized rubber provided by the invention, methyl vinyl phenyl silicone rubber with the molecular weight of 50-65 ten thousand is preferable.
According to the anti-fatigue damping vulcanized rubber provided by the invention, preferably, the white carbon black comprises one or two of fumed silica and precipitated silica.
According to the anti-fatigue damping vulcanized rubber provided by the invention, preferably, the plasticizer comprises dioctyl phthalate (DOP) and/or aromatic hydrocarbon oil.
According to the anti-fatigue damping vulcanized rubber provided by the invention, preferably, the vulcanizing agent comprises any one or more of dicumyl peroxide (DCP), di-tert-butyl peroxide (DTBP), 2, 5-dimethyl-2, 5-bis (tert-butylperoxy) hexane or Benzoyl Peroxide (BPO).
According to the anti-fatigue damping vulcanized rubber provided by the invention, preferably, the accelerator is one or two of N, N '-dicyclohexyl-2-benzothiazole sulfenamide (DZ) and N, N' -tetramethyl dithio-amine (TMTD).
In another aspect, the present invention provides a method for preparing an anti-fatigue damping vulcanized rubber, which comprises:
Placing 60-100 parts of chlorinated butyl rubber and 10-50 parts of trans-1, 4-polyisoprene rubber into a kneader for stirring, then sequentially adding 1-4 parts of zinc oxide, 1-3 parts of stearic acid, 0.5-2 parts of accelerator, 2-5 parts of plasticizer, 20-50 parts of white carbon black and 0.5-2 parts of sulfur component, and discharging after mixing to obtain a damping filler master batch mixing material;
Cooling the damping filler master batch mixture to room temperature, and standing to obtain damping filler master batch;
According to parts by weight, 80-120 parts of phenyl silicone rubber is placed in a kneader for stirring, then 10-40 parts of white carbon black is added for mixing, 10-30 parts of damping filler masterbatch and 1-4 parts of plasticizer are added after mixing, and the mixture is discharged after continuous mixing, so as to obtain a mixed rubber;
And cooling the rubber compound to room temperature, adding 1-2 parts of vulcanizing agent, standing the thin through piece on an open mill, and vulcanizing to obtain the anti-fatigue damping vulcanized rubber.
According to the preparation method provided by the invention, the step of adding the white carbon black is preferably carried out by adding 10-40 parts of white carbon black in multiple times, wherein the multiple times of adding are carried out by more than two times.
According to the preparation method provided by the invention, preferably, 1-2 parts of vulcanizing agent is added, and the mixture is placed for more than 24 hours after the sheet is thinned and discharged on an open mill. More preferably, 1 to 2 parts of vulcanizing agent are added and the mixture is placed for 24 to 72 hours after the sheet is thinly discharged on an open mill.
According to the preparation method provided by the invention, preferably, the vulcanization comprises the following specific operations: the rubber compound is placed on a flat vulcanizing machine, vulcanized for 8-15 minutes at 160-180 ℃, and then placed in a blast oven for vulcanization for 1.5-2.5 hours at 190-210 ℃ to obtain the anti-fatigue damping vulcanized rubber. More preferably, the vulcanization comprises the following specific operations: the rubber compound is placed on a flat vulcanizing machine, vulcanized for 10 minutes at 170 ℃, and then placed in a blast oven for vulcanization for 2 hours at 200 ℃ to obtain the anti-fatigue damping vulcanized rubber.
According to the preparation method provided by the invention, preferably, the damping filler masterbatch compound is cooled to room temperature and then is parked for more than 24 hours. More preferably, the damping filler masterbatch compound is cooled to room temperature and then parked for 24-72 hours.
Compared with the prior art, the invention has the following beneficial effects:
According to the invention, the trans-1, 4-polyisoprene rubber and the chlorinated butyl rubber are introduced into a phenyl silicone rubber system in a damping filler master batch mode, so that the fatigue resistance of the material can be greatly improved, and the prepared vulcanized rubber material has good mechanical properties, fatigue resistance and damping properties.
Detailed Description
The following describes specific embodiments of the present invention in detail. It should be understood that the detailed description and specific examples, while indicating and illustrating the invention, are not intended to limit the invention.
The endpoints and any values of the ranges disclosed herein are not limited to the precise range or value, and are understood to encompass values approaching those ranges or values. For numerical ranges, one or more new numerical ranges may be found between the endpoints of each range, between the endpoint of each range and the individual point value, and between the individual point value, in combination with each other, and are to be considered as specifically disclosed herein.
In the whole invention, the content of each component is weight part unless specified.
Example 1
The anti-fatigue damping vulcanized rubber provided by the embodiment comprises the following raw materials in parts by weight:
80 parts of phenyl silicone rubber;
20 parts of damping filler masterbatch;
35 parts of white carbon black;
2 parts of plasticizer DOP;
1 part of vulcanizing agent DCP;
Wherein, the damping filler masterbatch is prepared from the following raw materials in parts by weight:
80 parts of chlorinated butyl rubber;
50 parts of trans-1, 4-polyisoprene rubber;
40 parts of white carbon black;
2 parts of plasticizer DOP;
2.5 parts of zinc oxide;
2 parts of stearic acid;
1 part of sulfur;
0.5 part of accelerator DZ.
The preparation method of the damping filler masterbatch of the embodiment comprises the following steps:
placing chlorinated butyl rubber and trans-1, 4-polyisoprene rubber into a kneader for stirring, then sequentially adding zinc oxide, stearic acid, an accelerator, a plasticizer, white carbon black and sulfur components, mixing and discharging to obtain a damping filler masterbatch;
and cooling the damping filler master batch mixture to room temperature, and standing for 24 hours to obtain the damping filler master batch.
The preparation method of the anti-fatigue damping vulcanized rubber comprises the following steps:
placing phenyl silicone rubber into a kneader for stirring, adding white carbon black in batches, adding damping filler masterbatch and plasticizer after mixing, and discharging after mixing uniformly to obtain a mixed rubber;
cooling the rubber compound to room temperature, adding a vulcanizing agent DCP, thinning and discharging sheets on an open mill, and standing for 24 hours;
And vulcanizing the rubber compound with the thin through piece on a flat vulcanizing machine at 170 ℃ for 10 minutes to obtain a semi-finished product, and vulcanizing the semi-finished product in a blast oven at 200 ℃ for 2 hours to obtain vulcanized rubber. The properties of the vulcanized rubber obtained in this example are shown in Table 1.
Example 2
The anti-fatigue damping vulcanized rubber provided by the embodiment comprises the following raw materials in parts by weight:
120 parts of phenyl silicone rubber;
30 parts of damping filler masterbatch;
35 parts of white carbon black;
2 parts of plasticizer DOP;
1 part of vulcanizing agent DCP;
Wherein, the damping filler masterbatch is prepared from the following raw materials in parts by weight:
90 parts of chlorinated butyl rubber;
10 parts of trans-1, 4-polyisoprene rubber;
40 parts of white carbon black;
2 parts of plasticizer DOP;
2.5 parts of zinc oxide;
2 parts of stearic acid;
1 part of sulfur;
0.5 part of accelerator DZ;
the preparation method of the damping filler masterbatch of the embodiment comprises the following steps:
placing chlorinated butyl rubber and trans-1, 4-polyisoprene rubber into a kneader for stirring, then sequentially adding zinc oxide, stearic acid, an accelerator, a plasticizer, white carbon black and sulfur components, mixing and discharging to obtain a damping filler masterbatch;
and cooling the damping filler master batch mixture to room temperature, and standing for 24 hours to obtain the damping filler master batch.
The preparation method of the anti-fatigue damping vulcanized rubber comprises the following steps:
placing phenyl silicone rubber into a kneader for stirring, adding white carbon black in batches, adding damping filler masterbatch and plasticizer after mixing, and discharging after mixing uniformly to obtain a mixed rubber;
cooling the rubber compound to room temperature, adding a vulcanizing agent DCP, thinning and discharging sheets on an open mill, and standing for 24 hours;
And vulcanizing the rubber compound with the thin through piece on a flat vulcanizing machine at 170 ℃ for 10 minutes to obtain a semi-finished product, and vulcanizing the semi-finished product in a blast oven at 200 ℃ for 2 hours to obtain vulcanized rubber. The properties of the vulcanized rubber obtained in this example are shown in Table 1.
Example 3
The anti-fatigue damping vulcanized rubber provided by the embodiment comprises the following raw materials in parts by weight:
80 parts of phenyl silicone rubber;
20 parts of damping filler masterbatch;
35 parts of white carbon black;
2 parts of plasticizer DOP;
1 part of vulcanizing agent DCP;
Wherein, the damping filler masterbatch is prepared from the following raw materials in parts by weight:
80 parts of chlorinated butyl rubber;
30 parts of trans-1, 4-polyisoprene rubber;
40 parts of white carbon black;
2 parts of plasticizer DOP;
2.5 parts of zinc oxide;
2 parts of stearic acid;
1 part of sulfur;
0.5 part of accelerator DZ.
The preparation method of the damping filler masterbatch of the embodiment comprises the following steps:
placing chlorinated butyl rubber and trans-1, 4-polyisoprene rubber into a kneader for stirring, then sequentially adding zinc oxide, stearic acid, an accelerator, a plasticizer, white carbon black and sulfur components, mixing and discharging to obtain a damping filler masterbatch;
and cooling the damping filler master batch mixture to room temperature, and standing for 24 hours to obtain the damping filler master batch.
The preparation method of the anti-fatigue damping vulcanized rubber comprises the following steps:
placing phenyl silicone rubber into a kneader for stirring, adding white carbon black in batches, adding damping filler masterbatch and plasticizer after mixing, and discharging after mixing uniformly to obtain a mixed rubber;
cooling the rubber compound to room temperature, adding a vulcanizing agent DCP, thinning and discharging sheets on an open mill, and standing for 24 hours;
And vulcanizing the rubber compound with the thin through piece on a flat vulcanizing machine at 170 ℃ for 10 minutes to obtain a semi-finished product, and vulcanizing the semi-finished product in a blast oven at 200 ℃ for 2 hours to obtain vulcanized rubber. The properties of the vulcanized rubber obtained in this example are shown in Table 1.
Comparative example 1
The vulcanized rubber provided in the comparative example comprises the following raw materials in parts by weight:
80 parts of phenyl silicone rubber;
35 parts of white carbon black;
2 parts of plasticizer DOP;
1 part of vulcanizing agent DCP;
the preparation method of the vulcanized rubber provided in this comparative example is as follows:
Placing phenyl silicone rubber into a kneader for stirring, then adding white carbon black in batches, adding a plasticizer after mixing, and discharging after mixing uniformly to obtain a rubber compound;
cooling the rubber compound to room temperature, adding a vulcanizing agent DCP, thinning and discharging sheets on an open mill, and standing for 24 hours;
And vulcanizing the rubber compound with the thin through piece on a flat vulcanizing machine at 170 ℃ for 10 minutes to obtain a semi-finished product, and vulcanizing the semi-finished product in a blast oven at 200 ℃ for 2 hours to obtain vulcanized rubber. The properties of the vulcanized rubber obtained in this comparative example are shown in Table 1.
Comparative example 2
The vulcanized rubber provided in the comparative example comprises the following raw materials in parts by weight:
80 parts of phenyl silicone rubber;
20 parts of damping filler masterbatch;
35 parts of white carbon black;
2 parts of plasticizer DOP;
1 part of vulcanizing agent DCP;
Wherein, the damping filler masterbatch is prepared from the following raw materials in parts by weight:
80 parts of chlorinated butyl rubber;
40 parts of white carbon black;
2 parts of plasticizer DOP;
2.5 parts of zinc oxide;
2 parts of stearic acid;
1 part of sulfur;
0.5 part of accelerator DZ.
The preparation method of the damping filler masterbatch of the comparative example is as follows:
Placing chlorinated butyl rubber into a kneader for stirring, sequentially adding zinc oxide, stearic acid, an accelerator, a plasticizer, white carbon black and sulfur components, mixing, and discharging to obtain a damping filler masterbatch;
and cooling the damping filler master batch mixture to room temperature, and standing for 24 hours to obtain the damping filler master batch.
The preparation method of the vulcanized rubber of the comparative example is as follows:
placing phenyl silicone rubber into a kneader for stirring, adding white carbon black in batches, adding damping filler masterbatch and plasticizer after mixing, and discharging after mixing uniformly to obtain a mixed rubber;
cooling the rubber compound to room temperature, adding a vulcanizing agent DCP, thinning and discharging sheets on an open mill, and standing for 24 hours;
And vulcanizing the rubber compound with the thin through piece on a flat vulcanizing machine at 170 ℃ for 10 minutes to obtain a semi-finished product, and vulcanizing the semi-finished product in a blast oven at 200 ℃ for 2 hours to obtain vulcanized rubber. The properties of the vulcanized rubber obtained in this comparative example are shown in Table 1.
Comparative example 3
The vulcanized rubber provided in the comparative example comprises the following raw materials in parts by weight:
80 parts of phenyl silicone rubber;
39.49 parts of white carbon black;
plasticizer DOP 2.22 parts;
8.99 parts of chlorinated butyl rubber;
5.2 parts of trans-1, 4-polyisoprene rubber
0.28 Parts of zinc oxide;
0.22 parts of stearic acid;
1.11 parts of vulcanizing agent DCP;
0.055 parts of accelerator DZ.
The preparation method of the vulcanized rubber of the comparative example is as follows:
Placing phenyl silicone rubber, chlorinated butyl rubber and trans-1, 4-polyisoprene rubber into a kneader for stirring, sequentially adding zinc oxide, stearic acid, an accelerator, a plasticizer and white carbon black components, mixing, and discharging to obtain a mixed rubber;
cooling the rubber compound to room temperature, adding a vulcanizing agent DCP, thinning and discharging sheets on an open mill, and standing for 24 hours;
And vulcanizing the rubber compound with the thin through piece on a flat vulcanizing machine at 170 ℃ for 10 minutes to obtain a semi-finished product, and vulcanizing the semi-finished product in a blast oven at 200 ℃ for 2 hours to obtain vulcanized rubber. The properties of the vulcanized rubber obtained in this comparative example are shown in Table 1.
Table 1 table of properties of the rubbers produced in each example and comparative example
The preferred embodiments of the present invention have been described in detail above, but the present invention is not limited to the specific details of the above embodiments, and various simple modifications can be made to the technical solution of the present invention within the scope of the technical concept of the present invention, and all the simple modifications belong to the protection scope of the present invention.
In addition, the specific features described in the above embodiments may be combined in any suitable manner without contradiction. The various possible combinations of the invention are not described in detail in order to avoid unnecessary repetition. Moreover, any combination of the various embodiments of the invention can be made without departing from the spirit of the invention, which should also be considered as disclosed herein.

Claims (8)

1. The anti-fatigue damping vulcanized rubber is characterized by comprising the following raw materials in parts by weight:
80-100 parts of phenyl silicone rubber;
15-25 parts of damping filler masterbatch;
10-40 parts of white carbon black;
1-4 parts of plasticizer;
1-2 parts of vulcanizing agent;
wherein, the damping filler masterbatch is prepared from the following components in parts by weight:
60-100 parts of chlorinated butyl rubber;
10-50 parts of trans-1, 4-polyisoprene rubber;
20-50 parts of white carbon black;
2-5 parts of plasticizer;
1-4 parts of zinc oxide;
1-3 parts of stearic acid;
0.5-2 parts of sulfur;
0.5-2 parts of an accelerator;
the accelerator is one or two of N, N '-dicyclohexyl-2-benzothiazole sulfenamide and N, N' -tetramethyl disulfide dithio carbonyl amine;
The preparation process of the damping filler masterbatch comprises the following steps: placing 60-100 parts of chlorinated butyl rubber and 10-50 parts of trans-1, 4-polyisoprene rubber into a kneader for stirring, then sequentially adding 1-4 parts of zinc oxide, 1-3 parts of stearic acid, 0.5-2 parts of accelerator, 2-5 parts of plasticizer, 20-50 parts of white carbon black and 0.5-2 parts of sulfur component, mixing, and discharging to obtain a damping filler master batch mixture; and cooling the damping filler master batch mixture to room temperature, and standing to obtain the damping filler master batch.
2. The fatigue resistance damping vulcanizate of claim 1, wherein the fatigue resistance damping vulcanizate comprises, in parts by weight: 30-40 parts of white carbon black.
3. The anti-fatigue damping vulcanized rubber according to claim 1, wherein the phenyl silicone rubber comprises 10-30mol% of phenyl, 0.05-0.3mol% of vinyl and 50-65 ten thousand of molecular weight.
4. The fatigue resistance damping vulcanizate of claim 1, wherein the white carbon black comprises one or both of fumed silica or precipitated silica.
5. The fatigue resistant damping vulcanizate of claim 1, wherein the plasticizer comprises dioctyl phthalate and/or aromatic oil.
6. The fatigue-resistant damping vulcanizate of claim 1, wherein the vulcanizing agent comprises one or more of dicumyl peroxide, di-t-butyl peroxide, 2, 5-dimethyl-2, 5-bis (t-butylperoxy) hexane, or benzoyl peroxide.
7. A method for preparing the anti-fatigue damping vulcanized rubber as set forth in claim 1, comprising the steps of:
Placing 60-100 parts of chlorinated butyl rubber and 10-50 parts of trans-1, 4-polyisoprene rubber into a kneader for stirring, then sequentially adding 1-4 parts of zinc oxide, 1-3 parts of stearic acid, 0.5-2 parts of accelerator, 2-5 parts of plasticizer, 20-50 parts of white carbon black and 0.5-2 parts of sulfur component, mixing, and discharging to obtain a damping filler master batch mixture; cooling the damping filler master batch mixture to room temperature, and standing to obtain damping filler master batch;
according to parts by weight, placing 80-100 parts of phenyl silicone rubber into a kneader for stirring, adding 10-40 parts of white carbon black for mixing, adding 15-25 parts of damping filler masterbatch and 1-4 parts of plasticizer after mixing, and discharging after continuing mixing to obtain a mixed rubber;
And cooling the rubber compound to room temperature, adding 1-2 parts of vulcanizing agent, standing the thin through piece on an open mill, and vulcanizing to obtain the anti-fatigue damping vulcanized rubber.
8. The method of claim 7, wherein the vulcanization comprises the following specific operations: the rubber compound is placed on a flat vulcanizing machine, vulcanized for 8-15 minutes at 160-180 ℃, and then placed in a blast oven for vulcanization for 1.5-2.5 hours at 190-210 ℃ to obtain the anti-fatigue damping vulcanized rubber.
CN202211441754.1A 2022-11-17 2022-11-17 Anti-fatigue damping vulcanized rubber and preparation method thereof Active CN115678281B (en)

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CN112210216A (en) * 2020-08-31 2021-01-12 四川中物材料股份有限公司 High-damping phenyl silicone rubber and preparation method and application thereof
CN113354885A (en) * 2021-07-06 2021-09-07 仝国磊 Melt and chemical modified material for neoprene and rubber support and preparation method thereof

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ATE350416T1 (en) * 2001-11-30 2007-01-15 Zeon Corp RUBBER COMPOSITION, VULCANIZABLE RUBBER COMPOSITION AND DAMPING RUBBER VULCANIATE
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Publication number Priority date Publication date Assignee Title
CN105566705A (en) * 2014-10-31 2016-05-11 三力士股份有限公司 TPI modified rubber V band
CN112210216A (en) * 2020-08-31 2021-01-12 四川中物材料股份有限公司 High-damping phenyl silicone rubber and preparation method and application thereof
CN113354885A (en) * 2021-07-06 2021-09-07 仝国磊 Melt and chemical modified material for neoprene and rubber support and preparation method thereof

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