CN112048184A - Low-temperature-resistant mixing silicone rubber - Google Patents

Low-temperature-resistant mixing silicone rubber Download PDF

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Publication number
CN112048184A
CN112048184A CN202010968396.4A CN202010968396A CN112048184A CN 112048184 A CN112048184 A CN 112048184A CN 202010968396 A CN202010968396 A CN 202010968396A CN 112048184 A CN112048184 A CN 112048184A
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weight
parts
silicone rubber
temperature
fly ash
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CN202010968396.4A
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毕春花
胡国伟
张要
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Yuanling Chengruixiang Powder Material Technology Co ltd
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Yuanling Chengruixiang Powder Material Technology Co ltd
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    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08LCOMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L83/00Compositions of macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon only; Compositions of derivatives of such polymers
    • C08L83/04Polysiloxanes
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K2201/00Specific properties of additives
    • C08K2201/014Additives containing two or more different additives of the same subgroup in C08K
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08LCOMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2205/00Polymer mixtures characterised by other features
    • C08L2205/02Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group
    • C08L2205/025Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group containing two or more polymers of the same hierarchy C08L, and differing only in parameters such as density, comonomer content, molecular weight, structure

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  • Chemical & Material Sciences (AREA)
  • Health & Medical Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Medicinal Chemistry (AREA)
  • Polymers & Plastics (AREA)
  • Organic Chemistry (AREA)
  • Compositions Of Macromolecular Compounds (AREA)

Abstract

The invention discloses low-temperature-resistant mixing silicone rubber, which comprises 120 parts by weight of raw vinyl silicone rubber 110-one, 20-30 parts by weight of modified fly ash, 30-50 parts by weight of white carbon black, 2-4 parts by weight of hydroxyl silicone oil, 6-9 parts by weight of vulcanizing agent, 0.8-1.2 parts by weight of promoter M and 0.3-0.6 part by weight of anti-aging agent NBC; wherein, the molecular weight of the raw vinyl silicone rubber is 49-53 ten thousand, and the mol percentage content of vinyl is 0.2% -0.8%. According to the invention, the special modified fly ash is added into the mixed silicone rubber and is combined with the corresponding formula, so that the low-temperature performance of the mixed silicone rubber below-60 ℃ is effectively improved, and the application range of the mixed silicone rubber is expanded.

Description

Low-temperature-resistant mixing silicone rubber
Technical Field
The invention belongs to the field of materials, and particularly relates to low-temperature-resistant mixing silicone rubber.
Background
The mixed silicon rubber has excellent heat resistance, cold resistance, dielectricity, ozone resistance, atmospheric aging resistance and other performances, and the outstanding performance of the silicon rubber is wide in use temperature and can be used for a long time under the temperature of minus 60 ℃ (or lower) to plus 250 ℃ (or higher). But the silicon rubber is not suitable for lower temperature, and the low temperature of aerospace, ultra-low temperature refrigerator and the like can reach-75 ℃ or even-100 ℃, and the existing silicon rubber can not adapt to the corresponding temperature, so that the application range of the silicon rubber is limited.
Disclosure of Invention
The invention discloses low-temperature-resistant mixed silicone rubber. According to the invention, the special modified fly ash is added into the mixed silicone rubber and is combined with the corresponding formula, so that the low-temperature performance of the mixed silicone rubber below-60 ℃ is effectively improved, and the application range of the mixed silicone rubber is expanded.
In order to solve the problems, the technical scheme adopted by the invention is as follows:
a low-temperature resistant mixing silicone rubber comprises 120 parts by weight of vinyl silicone rubber crude rubber 110-30 parts by weight of modified fly ash, 30-50 parts by weight of white carbon black, 2-4 parts by weight of hydroxyl silicone oil, 6-9 parts by weight of vulcanizing agent, 0.8-1.2 parts by weight of accelerator M and 0.3-0.6 part by weight of anti-aging agent NBC;
wherein, the molecular weight of the raw vinyl silicone rubber is 49-53 ten thousand, and the mol percentage content of vinyl is 0.2% -0.8%.
The further improvement comprises 110 parts of vinyl silicone rubber crude rubber, 30 parts of modified fly ash, 30 parts of white carbon black, 4 parts of hydroxyl silicone oil, 6 parts of vulcanizing agent, 0.8 part of accelerator M and 0.6 part of anti-aging agent NBC.
The further improvement comprises 120 parts of vinyl silicone rubber crude rubber, 20 parts of modified fly ash, 50 parts of white carbon black, 2 parts of hydroxyl silicone oil, 9 parts of vulcanizing agent, 2.2 parts of accelerator M and 0.3 part of anti-aging agent NBC.
The further improvement comprises 115 parts by weight of raw vinyl silicone rubber, 25 parts by weight of modified fly ash, 35 parts by weight of white carbon black, 3 parts by weight of hydroxyl silicone oil, 7 parts by weight of vulcanizing agent, 1 parts by weight of accelerator M and 0.4 part by weight of anti-aging agent NBC.
Further improvement, the manufacturing method of the modified fly ash is as follows:
step one, grinding 100 parts by weight of fly ash to 5000-6000 meshes, and then treating for 2 hours at the temperature of 1MPa and 200 ℃;
step two, adding 3 parts by weight of silane coupling agent and 1 part by weight of stearic acid, stirring and uniformly mixing for 40min at the temperature of 80 ℃;
and step three, adding 10 parts by weight of polyethylene, uniformly mixing, and then sending into an extruder for extrusion at 180 ℃ to obtain the modified fly ash.
In a further improvement, the vulcanizing agent is tetramethylthiuram disulfide or sulfur.
Further improvement, the manufacturing method is as follows:
step one), uniformly mixing 120 parts by weight of raw vinyl silicone rubber 110-120 parts by weight of modified fly ash and 30-50 parts by weight of white carbon black, and then adding the mixture into a vacuum kneader for combination, wherein the kneading temperature is 105 ℃;
step two), adding 2-4 parts by weight of hydroxyl silicone oil, 0.8-1.2 parts by weight of accelerator M and 0.3-0.6 part by weight of anti-aging agent NBC, then vacuumizing until the vacuum degree is 0.01-0.08MPa, heating to 148 ℃, and continuing to mill until the materials are uniformly mixed;
step three), adding 6-9 parts by weight of vulcanizing agent to carry out high-temperature vulcanization at 160-170 ℃ to prepare the low-temperature resistant mixed silicone rubber.
Adopt the produced beneficial effect of above-mentioned technical scheme to lie in:
according to the invention, the special modified fly ash is added into the mixed silicone rubber and is combined with the corresponding formula, so that the low-temperature performance of the mixed silicone rubber below-60 ℃ is effectively improved, and the application range of the mixed silicone rubber is expanded.
Detailed Description
For purposes of clarity and a complete description of the present invention, and to provide further clarity and understanding of the objects, technical solutions and advantages thereof, it is to be understood that the terms "center", "vertical", "lateral", "up", "down", "front", "back", "left", "right", "vertical", "horizontal", "top", "bottom", "inner", "outer", and the like are used in an illustrative, positional or other orientation, and are used for convenience in describing and simplifying the present invention, but do not indicate or imply that the device or element being referred to must have a particular orientation, be constructed and operated in a particular orientation, and therefore should not be considered as limiting the present invention.
Example 1
The low-temperature-resistant mixed silicone rubber comprises 110 parts by weight of raw vinyl silicone rubber, 30 parts by weight of modified fly ash, 30 parts by weight of white carbon black, 4 parts by weight of hydroxy silicone oil, 6 parts by weight of vulcanizing agent, 0.8 part by weight of accelerator M and 0.6 part by weight of anti-aging agent NBC.
The manufacturing method comprises the following steps:
step one), uniformly mixing raw vinyl silicone rubber, modified fly ash and white carbon black, and then adding the mixture into a vacuum kneading machine for combination, wherein the kneading temperature is 105 ℃;
step two), adding hydroxyl silicone oil, an accelerator M and an anti-aging agent NBC, then vacuumizing until the vacuum degree is 0.01-0.08MPa, heating to 148 ℃, and continuing to mill until the materials are uniformly mixed;
and step three), adding a vulcanizing agent to vulcanize at the high temperature of 160-170 ℃ to prepare the low-temperature resistant mixed silicone rubber.
The preparation method of the modified fly ash is as follows:
step one, grinding 100 parts by weight of fly ash to 5000-6000 meshes, and then treating for 2 hours at the temperature of 1MPa and 200 ℃;
step two, adding 3 parts by weight of silane coupling agent and 1 part by weight of stearic acid, stirring and uniformly mixing for 40min at the temperature of 80 ℃;
and step three, adding 10 parts by weight of polyethylene, uniformly mixing, and then sending into an extruder for extrusion at 180 ℃ to obtain the modified fly ash.
Example 2
The low-temperature-resistant mixing silicone rubber comprises 120 parts by weight of raw vinyl silicone rubber, 20 parts by weight of modified fly ash, 50 parts by weight of white carbon black, 2 parts by weight of hydroxy silicone oil, 9 parts by weight of vulcanizing agent, 2 parts by weight of accelerator M.2 and 0.3 part by weight of anti-aging agent NBC.
Example 3
The low-temperature-resistant mixed silicone rubber comprises 115 parts by weight of raw vinyl silicone rubber, 25 parts by weight of modified fly ash, 35 parts by weight of white carbon black, 3 parts by weight of hydroxy silicone oil, 7 parts by weight of vulcanizing agent, 1 parts by weight of accelerator M and 0.4 part by weight of anti-aging agent NBC.
Comparative example 1
The low-temperature resistant mixed silicone rubber comprises 115 parts by weight of raw vinyl silicone rubber, 25 parts by weight of fly ash, 35 parts by weight of white carbon black, 3 parts by weight of hydroxy silicone oil, 7 parts by weight of vulcanizing agent, 1 parts by weight of accelerator M, and 0.4 part by weight of anti-aging agent NBC.
The procedure for the preparation of examples 1-3 is as follows:
grinding methyl vinyl silicone rubber, white carbon black and polytetrafluoroethylene into powder, uniformly mixing, putting into a kneader, and adding hydroxyl silicone oil and a tackifier;
step two, vacuumizing, wherein the vacuum degree is set to be minus 0.03 +/-0.01 MPa, the vacuumizing time is 25min, after vacuumizing is finished, adding aluminum tripolyphosphate, cerium powder and molybdenum powder, heating to 135 ℃, and secondarily vacuumizing, wherein the vacuum degree is set to be minus 0.01 +/-0.01 MPa, and the vacuumizing time is 60min to obtain a sizing material; the temperature rise rate at the time of temperature rise was 2.5 ℃/min
And step three, pouring the rubber material into a mold, and cooling and forming.
The detection data of the examples 1-3 and the existing product are as follows at a low temperature of-80 ℃:
Figure BDA0002683177550000041
finally, it should be noted that: the above examples are only intended to illustrate the technical solution of the present invention, but not to limit it; although the present invention has been described in detail with reference to the foregoing embodiments, it will be understood by those of ordinary skill in the art that: the technical solutions described in the foregoing embodiments may still be modified, or some technical features may be equivalently replaced; and such modifications or substitutions do not depart from the spirit and scope of the corresponding technical solutions of the embodiments of the present invention.

Claims (7)

1. The low-temperature-resistant mixing silicone rubber is characterized by comprising 120 parts by weight of raw vinyl silicone rubber 110-one, 20-30 parts by weight of modified fly ash, 30-50 parts by weight of white carbon black, 2-4 parts by weight of hydroxyl silicone oil, 6-9 parts by weight of vulcanizing agent, 0.8-1.2 parts by weight of accelerator M and 0.3-0.6 part by weight of anti-aging agent NBC;
wherein, the molecular weight of the raw vinyl silicone rubber is 49-53 ten thousand, and the mol percentage content of vinyl is 0.2% -0.8%.
2. The low-temperature-resistant compounded silicone rubber according to claim 1, comprising 110 parts by weight of raw vinyl silicone rubber, 30 parts by weight of modified fly ash, 30 parts by weight of white carbon black, 4 parts by weight of hydroxy silicone oil, 6 parts by weight of vulcanizing agent, 0.8 part by weight of accelerator M, and 0.6 part by weight of antioxidant NBC.
3. The low-temperature-resistant compounded silicone rubber according to claim 1, comprising 120 parts by weight of raw vinyl silicone rubber, 20 parts by weight of modified fly ash, 50 parts by weight of white carbon black, 2 parts by weight of hydroxy silicone oil, 9 parts by weight of vulcanizing agent, 2.2 parts by weight of accelerator m, and 0.3 part by weight of antioxidant NBC.
4. The low-temperature-resistant compounded silicone rubber according to claim 1, comprising 115 parts by weight of raw vinyl silicone rubber, 25 parts by weight of modified fly ash, 35 parts by weight of white carbon black, 3 parts by weight of hydroxy silicone oil, 7 parts by weight of vulcanizing agent, 1 parts by weight of accelerator M, and 0.4 part by weight of anti-aging agent NBC.
5. The low-temperature-resistant mixing silicone rubber according to claim 1, wherein the preparation method of the modified fly ash is as follows:
step one, grinding 100 parts by weight of fly ash to 5000-6000 meshes, and then treating for 2 hours at the temperature of 1MPa and 200 ℃;
step two, adding 3 parts by weight of silane coupling agent and 1 part by weight of stearic acid, stirring and uniformly mixing for 40min at the temperature of 80 ℃;
and step three, adding 10 parts by weight of polyethylene, uniformly mixing, and then sending into an extruder for extrusion at 180 ℃ to obtain the modified fly ash.
6. The low temperature resistant compounded silicone rubber according to claim 1, wherein the vulcanizing agent is tetramethylthiuram disulfide or sulfur.
7. The low-temperature resistant compounded silicone rubber according to claim 1, wherein the production method is as follows:
step one), uniformly mixing 120 parts by weight of raw vinyl silicone rubber 110-120 parts by weight of modified fly ash and 30-50 parts by weight of white carbon black, and then adding the mixture into a vacuum kneader for combination, wherein the kneading temperature is 105 ℃;
step two), adding 2-4 parts by weight of hydroxyl silicone oil, 0.8-1.2 parts by weight of accelerator M and 0.3-0.6 part by weight of anti-aging agent NBC, then vacuumizing until the vacuum degree is 0.01-0.08MPa, heating to 148 ℃, and continuing to mill until the materials are uniformly mixed;
step three), adding 6-9 parts by weight of vulcanizing agent to carry out high-temperature vulcanization at 160-170 ℃ to prepare the low-temperature resistant mixed silicone rubber.
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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114231037A (en) * 2021-11-09 2022-03-25 沅陵县成瑞祥粉体材料科技有限公司 Liquid conductive silicone rubber and preparation method thereof

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CN101824168A (en) * 2009-03-03 2010-09-08 柳州市圣诺科技有限公司 Method for preparing modified natural rubber by replacing carbon black with activated pulverized fuel ash
CN103013130A (en) * 2012-12-30 2013-04-03 江苏天辰硅材料有限公司 Silicon rubber and preparation method thereof
CN104497582A (en) * 2014-12-17 2015-04-08 苏州锦腾电子科技有限公司 Low-temperature-resistant silicon rubber and preparation method thereof
CN107446358A (en) * 2017-09-11 2017-12-08 江苏天辰新材料股份有限公司 A kind of low temperature resistant electrically insulating silicone rubber and preparation method thereof
CN108641370A (en) * 2018-03-30 2018-10-12 天长市荣盛有机硅科技有限公司 A kind of high-strength high temperature-resistant silicon rubber composite material

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CN103013130A (en) * 2012-12-30 2013-04-03 江苏天辰硅材料有限公司 Silicon rubber and preparation method thereof
CN104497582A (en) * 2014-12-17 2015-04-08 苏州锦腾电子科技有限公司 Low-temperature-resistant silicon rubber and preparation method thereof
CN107446358A (en) * 2017-09-11 2017-12-08 江苏天辰新材料股份有限公司 A kind of low temperature resistant electrically insulating silicone rubber and preparation method thereof
CN108641370A (en) * 2018-03-30 2018-10-12 天长市荣盛有机硅科技有限公司 A kind of high-strength high temperature-resistant silicon rubber composite material

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114231037A (en) * 2021-11-09 2022-03-25 沅陵县成瑞祥粉体材料科技有限公司 Liquid conductive silicone rubber and preparation method thereof

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Application publication date: 20201208