CN102424724A - Preparation method for gas phase method silicone rubber compound - Google Patents

Preparation method for gas phase method silicone rubber compound Download PDF

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CN102424724A
CN102424724A CN2011103808670A CN201110380867A CN102424724A CN 102424724 A CN102424724 A CN 102424724A CN 2011103808670 A CN2011103808670 A CN 2011103808670A CN 201110380867 A CN201110380867 A CN 201110380867A CN 102424724 A CN102424724 A CN 102424724A
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kneader
nitrogen
rubber
preparation
carrying
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CN102424724B (en
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任北军
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CHUZHOU JUNYUE HIGH POLYMER NEW MATERIAL Co Ltd
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CHUZHOU JUNYUE HIGH POLYMER NEW MATERIAL Co Ltd
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Abstract

The present invention discloses a preparation method for a gas phase method silicone rubber compound. The method comprises: adding raw rubber of the silicon rubber, gas phase method white carbon black, hydroxyl silicone oil, hydrogen-containing silicone oil and zinc stearate to a kneader; carrying out mixing and forming at a room temperature; carrying out vacuum pumping for the kneader for 4-6 minutes, and introducing nitrogen to the kneader for 13-17 minutes; then carrying out vacuum pumping for the kneader until the vacuum degree inside the kneader is more than -0.07 MPa, and introducing the nitrogen to the kneader for 13-17 minutes; continuously introducing the nitrogen to the kneader, wherein the nitrogen flow is maintained to more than 10 L/min; heating the temperature to 165-175 DEG C, holding the temperature for 2-3 hours; carrying out vacuum pumping for 8-12 minutes, and discharging the rubber; then carrying out treatments of cooling, roll banding, sheet discharging and filtering to obtain the product. According to the present invention, the process of the method of the present invention is simple; the product quality is high; the nitrogen is introduced during the whole process to protect the rubber mixing process, such that the concentration of the flammable and explosive gases is substantially reduced, the flammable and explosive gases are squeezed and discharged from the kneader, and the explosion caused by the static spark generated by the rubber mixing is prevented.

Description

A kind of preparation method of vapor phase process silicon rubber gross rubber
Technical field:
The invention belongs to vapor phase process silicon rubber gross rubber manufacturing technology field, exactly is a kind of preparation method of vapor phase process silicon rubber gross rubber.
Background technology:
At present, silicon rubber gross rubber produces CH when the heat refining because of it 3OH, CH 3CH 3Inflammable gas such as OH and very easily blast is very dangerous when therefore producing bring considerable influence can for the safety of enterprise, and product quality is difficult for guaranteeing, operator's personnel safety and quality product caused very big disadvantageous effect.Thereby, be badly in need of finding a kind of method of effective assurance vapor phase process silicon rubber gross rubber heat refining process, thereby solve refining glue safety-problems.
Summary of the invention:
The object of the invention is exactly in order to remedy the defective of prior art, provides the alloy ornament mould of a kind of high thixotropic that has, good physical and mechanical properties, high heat resistance to use the vapor phase process silicon rubber gross rubber.
The present invention realizes through following technical scheme:
A kind of preparation method of silicon rubber gross rubber is characterized in that may further comprise the steps:
A, in kneader, add raw-silastic continuously, thermal silica, hydroxy silicon oil, containing hydrogen silicone oil and Zinic stearas, the normal temperature mixing and molding;
B, kneader vacuumized 4-6 minute after, filled nitrogen 13-17 minute to kneader, vacuumize again that vacuum tightness reaches in kneader-more than the 0.07MPa, filled again nitrogen 13-17 minute;
C, continuation keep in kneader, charging into nitrogen, and nitrogen flow remains on more than the 10L/min, is warmed up to 165-175 ℃ again, are incubated after 2-3 hour, and plastic emitting after vacuum 8-12 minute more promptly gets product after cooling, bag roller, slice, filtration.
A kind of preparation method of silicon rubber gross rubber is characterized in that: before being warmed up to 165-175 ℃, need open the vent valve on the kneader cylinder cap, so that nitrogen is in time discharged the methyl alcohol that produces in the machine, ethanol gas in the machine.
A kind of preparation method of silicon rubber gross rubber is characterized in that: during the plastic emitting initial vacuum, close vent valve, the adjustment nitrogen valve charges in the machine with half the flow.
A kind of preparation method of silicon rubber gross rubber is characterized in that: the weight part of described each raw material is: raw-silastic continuously 800-1200, thermal silica 380-480, hydroxy silicon oil 35-55, containing hydrogen silicone oil 6-10, Triple Pressed Stearic Acid 4-8.
Beneficial effect of the present invention is:
Figure 2011103808670100002DEST_PATH_IMAGE001
Technology of the present invention is simple, and quality product is high, and through omnidistance inflated with nitrogen protection mixing process, the concentration that has greatly reduced flammable explosive gas with and it is squeezed to discharge kneader inner, prevent because the static sparking that refining glue produces is explosion caused.
Embodiment
(1) main raw material(s)
Gather ethylene methacrylic radical siloxane (raw-silastic continuously), molecular weight 65-75 ten thousand, the silicon industry company of containing is closed in Zhejiang;
WHITE CARBON BLACK: QS25, day Bender mountain; Hydroxy silicon oil, the Hongyuan, Yangzhou; Containing hydrogen silicone oil: Zhejiang San Men; Zinic stearas, Singapore.
(2) proportioning of the special-purpose rubber unvulcanizate of gas phase transparent silicon rubber nipple
The name of an article Consumption (mass parts)
Raw-silastic continuously 100
WHITE CARBON BLACK 48
Hydroxy silicon oil 4.5
Containing hydrogen silicone oil 0.8
Zinic stearas 0.6
(2) the main manufacturing and processing equipment of the special-purpose rubber unvulcanizate of gas phase transparent silicon rubber nipple
Equipment Model The place of production
Two roller mills 16 cun Morning twilight rubber machinery plant, Wuxi
Kneader 500L Jiangsu prosperous and powerful kneader factory
Vulcanizing press 25 tons Taizhou
(3) plant and instrument
Detecting instrument equipment mainly contains: sclerometer, reisilometer, electronic tensile machine etc.
Equipment Model The place of production
Sclerometer LX-A Jiangdu Xin Zhenwei test machines Ltd
Reisilometer WTD-0.5 Jiangdu Xin Zhenwei test machines Ltd
Electronic tensile machine ? Jiangdu Xin Zhenwei test machines Ltd
(4) specimen preparation
A kind of preparation method of silicon rubber gross rubber is characterized in that may further comprise the steps:
A, in kneader, add raw-silastic continuously, thermal silica, hydroxy silicon oil, containing hydrogen silicone oil and Zinic stearas, the normal temperature mixing and molding;
B, kneader vacuumized 5 minutes after, filled nitrogen 15 minutes to kneader, vacuumize again that vacuum tightness reaches in kneader-more than the 0.07MPa, filled nitrogen again 15 minutes;
C, continuation keep in kneader, charging into nitrogen, and nitrogen flow remains on more than the 10L/min, is warmed up to 170 ℃ again, are incubated after 2-3 hour, and vacuum plastic emitting after 10 minutes more promptly gets product after cooling, bag roller, slice, filtration.
A kind of preparation method of silicon rubber gross rubber is characterized in that: before being warmed up to 170 ℃, need open the vent valve on the kneader cylinder cap, so that nitrogen is in time discharged the methyl alcohol that produces in the machine, ethanol gas in the machine.
A kind of preparation method of silicon rubber gross rubber is characterized in that: during the plastic emitting initial vacuum, close vent valve, the adjustment nitrogen valve charges in the machine with half the flow.
2, performance test
Sample cure conditions: 170 ℃ * 10min
GB/T 531-1999 test is pressed in the detection of physicals property, hardness; Pull apart tensile strength and elongation, tear strength is tested by GB/T 528-1998.Test data sees the following form.
 
Figure 2011103808670100002DEST_PATH_IMAGE003
(5) result and discussion
1, uses the heat refining preparation method of omnidistance inflated with nitrogen protection, in the heat refining process, the quick-fried phenomenon of glue does not take place.
2, it should be noted that and be warmed up to before 170 ℃, must could guarantee that like this kneader does not have the air of remnants through vacuum → fill nitrogen → vacuum → fill the flow process of nitrogen → start → intensification.
3, in addition, driving part will keep excellent sealing property between the rotating shaft of kneader cylinder body and stirring arm, can not leak gas, and prevents air admission, and the oxygen of air is very easily combustion-supporting, and it is quick-fried to produce glue.
4, in the heat refining process, will guarantee the above kneader of flow, especially 1000L of nitrogen, nitrogen flow is not less than 10L/min.
When 5, starting shooting, need open the vent valve on the cylinder cap, so that nitrogen is in time discharged the methyl alcohol that produces in the machine, ethanol gas in the machine.
6, this heat refining technology has guaranteed the comprehensive physicals of product preferably, makes product have excellent ground use value.
(6) conclusion
Technology of the present invention is simple, and quality product is high, and through omnidistance inflated with nitrogen protection mixing process, the concentration that has greatly reduced flammable explosive gas with and it is squeezed to discharge kneader inner, prevent because the static sparking that refining glue produces is explosion caused.

Claims (4)

1. the preparation method of a silicon rubber gross rubber is characterized in that may further comprise the steps:
A, in kneader, add raw-silastic continuously, thermal silica, hydroxy silicon oil, containing hydrogen silicone oil and Zinic stearas, the normal temperature mixing and molding;
B, kneader vacuumized 4-6 minute after, filled nitrogen 13-17 minute to kneader, vacuumize again that vacuum tightness reaches in kneader-more than the 0.07MPa, filled again nitrogen 13-17 minute;
C, continuation keep in kneader, charging into nitrogen, and nitrogen flow remains on more than the 10L/min, is warmed up to 165-175 ℃ again, are incubated after 2-3 hour, and plastic emitting after vacuum 8-12 minute more promptly gets product after cooling, bag roller, slice, filtration.
2. the preparation method of a silicon rubber gross rubber is characterized in that: before being warmed up to 165-175 ℃, need open the vent valve on the kneader cylinder cap, so that nitrogen is in time discharged the methyl alcohol that produces in the machine, ethanol gas in the machine.
3. the preparation method of a silicon rubber gross rubber is characterized in that: during the plastic emitting initial vacuum, close vent valve, adjust nitrogen valve, charge in the machine with half the flow.
4. the preparation method of a silicon rubber gross rubber, it is characterized in that: the weight part of described each raw material is: raw-silastic continuously 800-1200, thermal silica 380-480, hydroxy silicon oil 35-55, containing hydrogen silicone oil 6-10, Triple Pressed Stearic Acid 4-8.
CN 201110380867 2011-11-25 2011-11-25 Preparation method for gas phase method silicone rubber compound Active CN102424724B (en)

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Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103834176A (en) * 2014-01-29 2014-06-04 迈高精细高新材料(深圳)有限公司 Method of preparing liquid silicone rubber
CN104109390A (en) * 2014-06-19 2014-10-22 滁州天成有机硅高分子材料有限公司 Food-contacting silicone rubber compound
CN107053512A (en) * 2017-05-06 2017-08-18 洛阳和梦科技有限公司 Multi-functional plastic cement processing unit (plant)
CN110204907A (en) * 2019-07-03 2019-09-06 常州大学怀德学院 It is a kind of to prevent technique on fire from explosion when mixing silicon rubber

Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101885919A (en) * 2010-07-15 2010-11-17 滁州君越高分子新材料有限公司 Gas-phase high-thixotropy silicon rubber compound
CN102061093A (en) * 2010-11-18 2011-05-18 东莞市耀盛硅材料科技有限公司 High-temperature resistant silicon rubber and preparation method thereof

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101885919A (en) * 2010-07-15 2010-11-17 滁州君越高分子新材料有限公司 Gas-phase high-thixotropy silicon rubber compound
CN102061093A (en) * 2010-11-18 2011-05-18 东莞市耀盛硅材料科技有限公司 High-temperature resistant silicon rubber and preparation method thereof

Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103834176A (en) * 2014-01-29 2014-06-04 迈高精细高新材料(深圳)有限公司 Method of preparing liquid silicone rubber
CN103834176B (en) * 2014-01-29 2017-01-18 迈高精细高新材料(深圳)有限公司 Method of preparing liquid silicone rubber
CN104109390A (en) * 2014-06-19 2014-10-22 滁州天成有机硅高分子材料有限公司 Food-contacting silicone rubber compound
CN107053512A (en) * 2017-05-06 2017-08-18 洛阳和梦科技有限公司 Multi-functional plastic cement processing unit (plant)
CN110204907A (en) * 2019-07-03 2019-09-06 常州大学怀德学院 It is a kind of to prevent technique on fire from explosion when mixing silicon rubber
CN110204907B (en) * 2019-07-03 2021-05-11 常州大学怀德学院 Process for preventing explosion and fire in silicon rubber mixing

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