CN103642245A - Silicone rubber preparation method - Google Patents

Silicone rubber preparation method Download PDF

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Publication number
CN103642245A
CN103642245A CN201310599429.2A CN201310599429A CN103642245A CN 103642245 A CN103642245 A CN 103642245A CN 201310599429 A CN201310599429 A CN 201310599429A CN 103642245 A CN103642245 A CN 103642245A
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China
Prior art keywords
silicon rubber
gas
mixing
rubber preparation
parts
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Pending
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CN201310599429.2A
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Chinese (zh)
Inventor
尤晓明
李洋
刘国华
张兰鹏
葛汝海
燕纪祥
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Shandong Yongtai Chemical Group Co Ltd
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Shandong Yongtai Chemical Group Co Ltd
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Priority to CN201310599429.2A priority Critical patent/CN103642245A/en
Publication of CN103642245A publication Critical patent/CN103642245A/en
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Abstract

The invention discloses a silicone rubber preparation method. The method comprises the following steps: mixing raw rubber of silicone rubber in a mixing mill, then orderly adding polyorganometallosiloxane, alkyloxy terminated polysiloxane, gas-phase white carbon black, hydroxyl silicone oil, methyl ethyl silicone oil and a heat-resistant addictive, fully mixing, and then subjecting the mixture to a sulfuration treatment so as to obtain the target silicone rubber. The silicone rubber produced by the preparation method provided by the invention overcomes the defects of bad high-temperature resistant and anti-aging performances of common silicone rubber; furthermore, hydroxyl silicone oil and methyl ethyl silicone oil are added so as to strengthen the anti-tearing performance of the silicone rubber; the prepared novel material has a better heat resistant performance, and is user-friendly.

Description

A kind of silicon rubber preparation method
Technical field
The present invention relates to silicon rubber preparation method technical field, particularly relate to a kind of silicon rubber preparation method.
Background technology
Silicon rubber is a kind of good specialty elastomer, it has good thermotolerance, low temperature resistant, insulativity, antidetonation, resistance to compression, wear-resistant and good biological nature, make it have range of application widely, such as building, communications and transportation, electronic apparatus, chemical industry, biomaterial and present aerospace material etc.Silicon rubber can be at-65 ℃~200 ℃ life-time service now, but along with scientific and technological development, its thermotolerance is had higher requirement, and present aeronautical and space technology requires silicon rubber life-time service at higher temperature, the resistance to elevated temperatures that further improves silicon rubber has very large meaning, in addition, in the situation that thermotolerance improves, the tear strength of silicon rubber also needs further perfect.Therefore need a kind of new silicon rubber preparation method, silicon rubber is being improved to some extent aspect thermotolerance, tear strength.
Summary of the invention
Object of the present invention is exactly to provide a kind of silicon rubber preparation method for the defect of above-mentioned existence.There is the poor defect of heat resistant in the ordinary silicon rubber that silicon rubber prepared by the present invention has overcome prior art, the tear strength that the hydroxy silicon oil adding and methylethyl silicone oil have increased silicon rubber, the novel material effect of preparing is better than original silicon rubber heat-resisting, easy to use.
A kind of silicon rubber preparation method technical scheme of the present invention is that step comprises:
(1) raw-silastic continuously is placed on mixing roll mixing, then adds successively polyorganometallosiloxane, alkoxy end-capped polysiloxane, gas-phase silica, hydroxy silicon oil, methylethyl silicone oil and heat-resisting additive fully mixing;
(2) the mixing product of step (1) is placed after 10~24 hours and on mixing roll, carried out back mixing, and add two two or five vulcanizing agents, in baking oven, vulcanize, oven temperature keeps 160 ℃~200 ℃, makes silicon rubber of the present invention.
In step (2), in baking oven, temperature is 180 ℃~200 ℃, sulfuration 4~5h.
Each raw material is by weight: 100 parts, silicon rubber, 100 parts of polyorganometallosiloxanes, 0~80 part of alkoxy end-capped polysiloxane, 10~20 parts of two two or five vulcanizing agents, 20~50 parts of gas-phase silicas, 1~5 part of methylethyl silicone oil, 1~5 part of hydroxy silicon oil, 1~10 part of heat-resisting additive.
Described silicon rubber is methyl vinyl silicone rubber, and heat-resisting additive is nano-stannic oxide.
Described gas-phase silica is common gas-phase silica or silanization gas-phase silica.
Preferably, described gas-phase silica is that silanization is processed hydrophobic type gas-phase silica.
The metallic element of described polyorganometallosiloxane is copper Cu, iron Fe, cerium Ce, vanadium Vi, titanium Ti.
Described polyorganometallosiloxane is pressed powder or the solution that is dissolved in organic solvent, organic solvent is methyl alcohol, ethanol, propyl alcohol, Virahol, butanols, isopropylcarbinol alcoholic solvent, one or more in benzene,toluene,xylene aromatic hydrocarbon solvent and ritalin, ethyl ester, propyl ester, butyl ester.
Described polyorganometallosiloxane is pressed powder, and its granularity is 200-2000 order.
Described alkoxy end-capped polysiloxane molecule formula is ROSi (CH3) 2 (OSi (CH3) 2) nR, n=0 ~ 20 wherein, and R is CH3, C2H5, a kind of in C6H5.
Beneficial effect of the present invention is: the heat-resisting additive nano-stannic oxide that the present invention uses belongs to rutile, has the features such as high-melting-point, Heat stability is good, corrosion-resistant, good mechanical stability.Hydroxy silicon oil and methylethyl silicone oil play Concentrative crosslinking in this composition, make it produce inhomogeneous Concentrative crosslinking, and the strong point that height of formation is crosslinked, has high tear strength.It is major function material that the present invention adopts solubility polyorganometallosiloxane, improve the intermiscibility (or dispersed) of additive in silicon rubber, thereby improve silicon rubber heat-resisting, through experimental verification, silicon rubber of the present invention can be used for a long time under the environment of 335-360 degree Celsius, and tear strength can reach 31.8KN/m.
embodiment:
In order to understand better the present invention, with specific examples, describe technical scheme of the present invention in detail below, but the present invention is not limited thereto.
Embodiment 1
A kind of silicon rubber preparation method of the present invention, contains following composition by weight: 100 parts, silicon rubber, 100 parts of polyorganometallosiloxanes, 50 parts of alkoxy end-capped polysiloxane, 11 parts of two two or five vulcanizing agents, 20 parts of gas-phase silicas, 4 parts of methylethyl silicone oil, 3 parts of hydroxy silicon oils, 3 parts of heat-resisting additives.
Described silicon rubber is methyl vinyl silicone rubber.
Described heat-resisting additive is nano-stannic oxide.
Described gas-phase silica is that silanization is processed hydrophobic type gas-phase silica.
The metallic element of described polyorganometallosiloxane is vanadium Vi.
Described polyorganometallosiloxane is the solution that is dissolved in organic solvent, organic solvent Virahol and dimethylbenzene aromatic hydrocarbon solvent.
Described alkoxy end-capped polysiloxane molecule formula is ROSi (CH3) 2 (OSi (CH3) 2) nR, n=16 wherein, and R can be CH3, C2H5, C6H5.
Silicon rubber of the present invention is prepared according to the following step:
(1) described raw-silastic continuously is placed on mixing roll mixing, then adds successively polyorganometallosiloxane, alkoxy end-capped polysiloxane, gas-phase silica, hydroxy silicon oil, methylethyl silicone oil and heat-resisting additive fully mixing;
(2) the mixing product of step (1) is placed after 10~24 hours and on mixing roll, carried out back mixing, and add two two or five vulcanizing agents, in baking oven, vulcanize, oven temperature keeps 160 ℃~200 ℃, makes silicon rubber of the present invention.
Through experimental verification, silicon rubber of the present invention can be used for a long time under the environment of 350-360 degree Celsius, and tear strength can reach 31.8KN/m.
Embodiment 2
A kind of silicon rubber preparation method of the present invention, contains following composition by weight: 100 parts, silicon rubber, 100 parts of polyorganometallosiloxanes, 80 parts of alkoxy end-capped polysiloxane, 10 parts of two two or five vulcanizing agents, 20 parts of gas-phase silicas, 5 parts of methylethyl silicone oil, 5 parts of hydroxy silicon oils, 8 parts of heat-resisting additives.
Described silicon rubber is methyl vinyl silicone rubber.
Described heat-resisting additive is nano-stannic oxide.
Described gas-phase silica is common gas-phase silica.
The metallic element of described polyorganometallosiloxane is cerium Ce.
Described polyorganometallosiloxane is pressed powder, and its granularity is 200-2000 order.
Described alkoxy end-capped polysiloxane molecule formula is ROSi (CH3) 2 (OSi (CH3) 2) nR, n=10 wherein, and R can be CH3, C2H5, C6H5.
Silicon rubber of the present invention is prepared according to the following step:
(1) described raw-silastic continuously is placed on mixing roll mixing, then adds successively polyorganometallosiloxane, alkoxy end-capped polysiloxane, gas-phase silica, hydroxy silicon oil, methylethyl silicone oil and heat-resisting additive fully mixing;
(2) the mixing product of step (1) is placed after 10~24 hours and on mixing roll, carried out back mixing, and add two two or five vulcanizing agents, in baking oven, vulcanize, oven temperature keeps 160 ℃~200 ℃, makes silicon rubber of the present invention.
Through experimental verification, silicon rubber of the present invention can be used for a long time under the environment of 335-350 degree Celsius, and tear strength can reach 30.6KN/m.
Embodiment 3
A kind of silicon rubber preparation method of the present invention, contains following composition by weight: 100 parts, silicon rubber, 100 parts of polyorganometallosiloxanes, 20 parts of alkoxy end-capped polysiloxane, 16 parts of two two or five vulcanizing agents, 30 parts of gas-phase silicas, 2 parts of methylethyl silicone oil, 5 parts of hydroxy silicon oils, 5 parts of heat-resisting additives.
Described silicon rubber is methyl vinyl silicone rubber.
Described heat-resisting additive is nano-stannic oxide.
Described gas-phase silica is that silanization is processed hydrophobic type gas-phase silica.
The metallic element of described polyorganometallosiloxane is copper Cu.
Described polyorganometallosiloxane is the solution that is dissolved in organic solvent, and organic solvent is benzene.
Described alkoxy end-capped polysiloxane molecule formula is ROSi (CH3) 2 (OSi (CH3) 2) nR, n=5 wherein, and R can be CH3, C2H5, C6H5.
Silicon rubber of the present invention is prepared according to the following step:
(1) described raw-silastic continuously is placed on mixing roll mixing, then adds successively polyorganometallosiloxane, alkoxy end-capped polysiloxane, gas-phase silica, hydroxy silicon oil, methylethyl silicone oil and heat-resisting additive fully mixing;
(2) the mixing product of step (1) is placed after 10~24 hours and on mixing roll, carried out back mixing, and add two two or five vulcanizing agents, in baking oven, vulcanize, oven temperature keeps 160 ℃~200 ℃, makes silicon rubber of the present invention.
Through experimental verification, silicon rubber of the present invention can be used for a long time under the environment of 335-350 degree Celsius, and tear strength can reach 31.3KN/m.

Claims (10)

1. a silicon rubber preparation method, is characterized in that, step comprises:
(1) raw-silastic continuously is placed on mixing roll mixing, then adds successively polyorganometallosiloxane, alkoxy end-capped polysiloxane, gas-phase silica, hydroxy silicon oil, methylethyl silicone oil and heat-resisting additive fully mixing;
(2) the mixing product of step (1) is placed after 10~24 hours and on mixing roll, carried out back mixing, and add two two or five vulcanizing agents, in baking oven, vulcanize, oven temperature keeps 160 ℃~200 ℃, makes silicon rubber of the present invention.
2. a kind of silicon rubber preparation method according to claim 1, is characterized in that, in step (2), in baking oven, temperature is 180 ℃~200 ℃, sulfuration 4~5h.
3. a kind of silicon rubber preparation method according to claim 1, it is characterized in that, each raw material is by weight: 100 parts, silicon rubber, 100 parts of polyorganometallosiloxanes, 0~80 part of alkoxy end-capped polysiloxane, 10~20 parts of two two or five vulcanizing agents, 20~50 parts of gas-phase silicas, 1~5 part of methylethyl silicone oil, 1~5 part of hydroxy silicon oil, 1~10 part of heat-resisting additive.
4. a kind of silicon rubber preparation method according to claim 1, is characterized in that, described silicon rubber is methyl vinyl silicone rubber, and heat-resisting additive is nano-stannic oxide.
5. a kind of silicon rubber preparation method according to claim 1, is characterized in that, described gas-phase silica is common gas-phase silica or silanization gas-phase silica.
6. a kind of silicon rubber preparation method according to claim 5, is characterized in that, described gas-phase silica is that silanization is processed hydrophobic type gas-phase silica.
7. a kind of silicon rubber preparation method according to claim 1, is characterized in that, the metallic element of described polyorganometallosiloxane is copper Cu, iron Fe, cerium Ce, vanadium Vi, titanium Ti.
8. a kind of silicon rubber preparation method according to claim 1, it is characterized in that, described polyorganometallosiloxane is pressed powder or the solution that is dissolved in organic solvent, organic solvent is methyl alcohol, ethanol, propyl alcohol, Virahol, butanols, isopropylcarbinol alcoholic solvent, one or more in benzene,toluene,xylene aromatic hydrocarbon solvent and ritalin, ethyl ester, propyl ester, butyl ester.
9. a kind of silicon rubber preparation method according to claim 1, is characterized in that, described polyorganometallosiloxane is pressed powder, and its granularity is 200-2000 order.
10. a kind of silicon rubber preparation method according to claim 1, is characterized in that, described alkoxy end-capped polysiloxane molecule formula is ROSi (CH3) 2 (OSi (CH3) 2) nR, n=0 ~ 20 wherein, R is CH3, C2H5, a kind of in C6H5.
CN201310599429.2A 2013-11-25 2013-11-25 Silicone rubber preparation method Pending CN103642245A (en)

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Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104761904A (en) * 2015-03-16 2015-07-08 芜湖荣基密封系统有限公司 Nano-titanium diboride-doped anti-corrosion silicone rubber cement used for preparing ultrathin rubber sealing layer and preparation method thereof
CN106751855A (en) * 2016-12-12 2017-05-31 芜湖集拓橡胶技术有限公司 The silicon rubber oil sealing material prescription of air inlet pipe
CN107337819A (en) * 2017-06-29 2017-11-10 福清市汇华塑胶制品有限公司 A kind of preparation method of elastomeric material
CN112322047A (en) * 2020-10-27 2021-02-05 宁波星箭航空机械制造有限公司 Supercharging pipe with high temperature resistance and preparation process thereof
CN112778763A (en) * 2020-12-28 2021-05-11 苏州楷蒙电子有限公司 Preparation method of heat-conducting silicone rubber material
CN113337119A (en) * 2021-05-27 2021-09-03 厦门汉升橡塑制品有限公司 Weather-resistant silicone rubber and preparation method thereof

Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101899214A (en) * 2010-04-19 2010-12-01 上海爱世博有机硅材料有限公司 Silicon rubber heat-resisting additive and method
CN102643550A (en) * 2012-04-28 2012-08-22 宜兴市聚金信化工有限公司 High-temperature-resistant silicon rubber additive and method

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101899214A (en) * 2010-04-19 2010-12-01 上海爱世博有机硅材料有限公司 Silicon rubber heat-resisting additive and method
CN102643550A (en) * 2012-04-28 2012-08-22 宜兴市聚金信化工有限公司 High-temperature-resistant silicon rubber additive and method

Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104761904A (en) * 2015-03-16 2015-07-08 芜湖荣基密封系统有限公司 Nano-titanium diboride-doped anti-corrosion silicone rubber cement used for preparing ultrathin rubber sealing layer and preparation method thereof
CN106751855A (en) * 2016-12-12 2017-05-31 芜湖集拓橡胶技术有限公司 The silicon rubber oil sealing material prescription of air inlet pipe
CN107337819A (en) * 2017-06-29 2017-11-10 福清市汇华塑胶制品有限公司 A kind of preparation method of elastomeric material
CN112322047A (en) * 2020-10-27 2021-02-05 宁波星箭航空机械制造有限公司 Supercharging pipe with high temperature resistance and preparation process thereof
CN112778763A (en) * 2020-12-28 2021-05-11 苏州楷蒙电子有限公司 Preparation method of heat-conducting silicone rubber material
CN113337119A (en) * 2021-05-27 2021-09-03 厦门汉升橡塑制品有限公司 Weather-resistant silicone rubber and preparation method thereof

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Application publication date: 20140319