CN102408725A - Silicone rubber applicable to microwave curing and preparation method thereof - Google Patents

Silicone rubber applicable to microwave curing and preparation method thereof Download PDF

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Publication number
CN102408725A
CN102408725A CN2011103539960A CN201110353996A CN102408725A CN 102408725 A CN102408725 A CN 102408725A CN 2011103539960 A CN2011103539960 A CN 2011103539960A CN 201110353996 A CN201110353996 A CN 201110353996A CN 102408725 A CN102408725 A CN 102408725A
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microwave
vulcanization
section
curing
warm air
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CN102408725B (en
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张洪起
王娟
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Tianjin Peng Ling group Limited by Share Ltd
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Tianjin Pengling Rubber Hose Co Ltd
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • B29C48/00—Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor
    • B29C48/25—Component parts, details or accessories; Auxiliary operations
    • B29C48/92—Measuring, controlling or regulating
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • B29C48/00—Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor
    • B29C48/25—Component parts, details or accessories; Auxiliary operations
    • B29C48/36—Means for plasticising or homogenising the moulding material or forcing it through the nozzle or die
    • B29C48/395—Means for plasticising or homogenising the moulding material or forcing it through the nozzle or die using screws surrounded by a cooperating barrel, e.g. single screw extruders
    • B29C48/397—Means for plasticising or homogenising the moulding material or forcing it through the nozzle or die using screws surrounded by a cooperating barrel, e.g. single screw extruders using a single screw
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • B29C2948/00—Indexing scheme relating to extrusion moulding
    • B29C2948/92—Measuring, controlling or regulating
    • B29C2948/92504—Controlled parameter
    • B29C2948/92561—Time, e.g. start, termination, duration or interruption
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • B29C2948/00—Indexing scheme relating to extrusion moulding
    • B29C2948/92—Measuring, controlling or regulating
    • B29C2948/92504—Controlled parameter
    • B29C2948/9258—Velocity
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • B29C2948/00—Indexing scheme relating to extrusion moulding
    • B29C2948/92—Measuring, controlling or regulating
    • B29C2948/92504—Controlled parameter
    • B29C2948/9258—Velocity
    • B29C2948/9259—Angular velocity
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • B29C2948/00—Indexing scheme relating to extrusion moulding
    • B29C2948/92—Measuring, controlling or regulating
    • B29C2948/92504—Controlled parameter
    • B29C2948/92704—Temperature
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • B29C2948/00—Indexing scheme relating to extrusion moulding
    • B29C2948/92—Measuring, controlling or regulating
    • B29C2948/92819—Location or phase of control
    • B29C2948/92857—Extrusion unit
    • B29C2948/92876—Feeding, melting, plasticising or pumping zones, e.g. the melt itself
    • B29C2948/92885—Screw or gear
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • B29C2948/00—Indexing scheme relating to extrusion moulding
    • B29C2948/92—Measuring, controlling or regulating
    • B29C2948/92819—Location or phase of control
    • B29C2948/92857—Extrusion unit
    • B29C2948/92876—Feeding, melting, plasticising or pumping zones, e.g. the melt itself
    • B29C2948/92895—Barrel or housing
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • B29C2948/00—Indexing scheme relating to extrusion moulding
    • B29C2948/92—Measuring, controlling or regulating
    • B29C2948/92819—Location or phase of control
    • B29C2948/92923—Calibration, after-treatment or cooling zone
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • B29C2948/00—Indexing scheme relating to extrusion moulding
    • B29C2948/92—Measuring, controlling or regulating
    • B29C2948/92819—Location or phase of control
    • B29C2948/92933—Conveying, transporting or storage of articles

Abstract

The invention relates to a silicone rubber applicable to microwave curing and a preparation method thereof. The composition of the silicone rubber comprises methylvinylsilicone rubber, carbon black, hydroxylsilicone oil, methylsilicone oil, white carbon black and C-224A curing agent. Matched with the speed of a microwave curing and traction section, a rubber tube is extruded out by a single screw extruder, and is then molded in a microwave curing mode; and in the microwave curing process, a one-section microwave and three-section hot-air curing device is used for microwave curing, and a two-section curing mode is used for molding. The invention meets the performance requirements of the finished product, and still has favorable product performance at the high temperature of 200 DEG C.

Description

A kind of Zylox and preparation method who is applicable to microwave vulcanization
Technical field
The present invention relates to the sebific duct technical field, particularly a kind of microwave vulcanization Zylox and preparation method who is applicable to little internal diameter.
Background technology
Sulfuration is a most important process step in the rubber item course of processing, and traditional vulcanization process is like the operational method by thermal conduction heating principle such as pressurization compression molding, the sulfuration of steam vulcanization jar, hot-air vulcanization, salt bath vulcanization.
At present, the extrusion type silicone rubber products adopts the sulfuration of steam vulcanization jar mostly, and the mode of this process using HTHP realizes vulcanization crosslinking.The sulfuration of steam vulcanization jar can be for vulcanizate provides higher pressure, so it has certain help to performance of products.But the straight type product that this vulcanization process is little to internal diameter, length is long is not best vulcanization, and product not only is difficult to be inserted in plug and puts, and the defective goods rate in the sulfidation is also very high.
Microwave vulcanization then is to be the vulcanization process of principal character with microwave heating, and its temperature is particularly suitable for vulcanizing the short extruded product endless vulcanization production line of flow process up to 250 ℃.Adopt microwave heating, equipment takes up an area of few (because of device length shortens), and curing cycle can shorten 1/3, and therefore manufacturing cost also reduces.The distinguishing feature of microwave vulcanization simultaneously is to have the fastest rate of heating and minimum energy consumption.
Cause owing to self property endured of Zylox is bad the straight type product of large diameter Zylox before extruding back, microwave vulcanization in the lateral traction process half-finished rounding property bad, then for the silicone rubber products of large diameter, the microwave vulcanization mode is not very suitable.But the straight type silicone rubber products that is embodied in internal diameter less than 20mm with the obvious advantage of microwave vulcanization technology.
Adopt the microwave vulcanization technology to substitute the prior steam sulfuration process internal diameter is carried out disposal molding less than the straight type silicone rubber products of 20mm, greatly reduce production cost, improved production efficiency; Microwave vulcanization combines with the hot blast sulfuration, can guarantee the technical requirements of silica gel sebific duct, can reduce the waste of energy again.
Summary of the invention
The object of the invention just provides a kind of microwave vulcanization Zylox and preparation method who is applicable to little internal diameter; Through rational formulating of recipe and technological design, thereby make little internal diameter silica gel product can adopt microwave vulcanization to carry out the effect that reaches High-efficient Production, hangs down waste material, hangs down the product stability of manpower and excellence.
The present invention adopts the Zylox that is fit to the microwave vulcanization prescription to realize the microwave vulcanization production of silica gel sebific duct with excellent technological process control.
The invention has the advantages that after the silica gel sebific duct is extruded and directly carry out microwave vulcanization that product is extruded with moulding has excellent continuity.
The present invention is mainly used in the little internal diameter full glue silicone tube of automobile upward pressure requirement at 0.7MPa～0.8MPa.
A kind of microwave vulcanization Zylox that is applicable to, component and mass fraction prescription are following:
Figure BDA0000106968850000021
The preparation method of Zylox of the present invention, sebific duct is that the speed that adopts single screw extrusion machine, cooperates microwave vulcanization to draw section carries out carrying out moulding through the mode of microwave vulcanization again after sebific duct is extruded; Concrete sulfidization molding technology controlling and process is following:
1) microwave vulcanization
Use one section microwave, three sections hot-air vulcanization equipment to carry out the microwave vulcanization moulding:
Microwave section temperature is controlled at 210 ℃～230 ℃, and one section temperature of warm air beating is 210 ℃～230 ℃, and two sections temperature of warm air beating are 210 ℃～230 ℃, and three sections temperature of warm air beating are 210 ℃～230 ℃, and pulling speed is controlled at 5～10m/min;
2) adopt the post vulcanization mode
Adopt the post cure mode of 120 ℃ * 2h after the microwave vulcanization.
Effect of the present invention: because sebific duct is the straight type silicone tube of full glue, adopt common silica gel extrusion way to cooperate the microwave vulcanization once shaped, the equipment of having given prominence to takes up an area of few (because of device length shortens), and curing cycle can shorten 1/3 advantage.For the Zylox of Shore A hardness in 65 to 75 hardness, select two two or four vulcanizing agents to add Zylox, solve it and in the microwave vulcanization process, produced the problem that micropore and surface blistering phenomenon influence performance; What select to be fit to extrudes pulling speed, avoids product phenomenon of complete cure and over cure not in the microwave vulcanization process.To sum up, adopt specific silicone rubber prescription cooperation microwave vulcanization can reach the effect of the product stability that when satisfying product performance, reaches High-efficient Production, low waste material, low manpower and excellence.
Embodiment
For a kind of silica gel sebific duct of full glue, require hardness 65 ± 5shore A, tensile strength >=7.5MPa, elongation >=200%; Changes in hardness ± 10 after the 200 ℃ * 70h thermal ageing, tensile strength changes ± 30%, and elongation change is in-40%.
Embodiment 1:
Figure BDA0000106968850000031
The sulfuration process parameter designing is following:
1), microwave section temperature is controlled at 210 ℃, 1 section temperature of warm air beating is 210 ℃, 2 sections temperature of warm air beating are 210 ℃, 3 sections temperature of warm air beating are 210 ℃.Pulling speed is controlled at 5m/min.
2), post cure: 120 ℃ * 2h.
Embodiment 2:
The silica gel prescription is following:
The sulfuration process parameter designing is following:
1), microwave section temperature is controlled at 220 ℃, 1 section temperature of warm air beating is 220 ℃, 2 sections temperature of warm air beating are 220 ℃, 3 sections temperature of warm air beating are 220 ℃.Pulling speed is controlled at 8m/min.
2), post cure: 120 ℃ * 2h.
Embodiment 3:
The silica gel prescription is following:
Figure BDA0000106968850000033
The sulfuration process parameter designing is following:
1), microwave section temperature is controlled at 230 ℃, 1 section temperature of warm air beating is 230 ℃, 2 sections temperature of warm air beating are 230 ℃, 3 sections temperature of warm air beating are 230 ℃.Pulling speed is controlled at 10m/min.
2), post cure: 120 ℃ * 2h.
Table 1: microwave vulcanization silicone tube performance
Figure BDA0000106968850000042
Through the above embodiments, can find out obviously that the present invention satisfies the end properties requirement, and under 200 ℃ of hot conditionss, still have good product performance.

Claims (2)

1. one kind is applicable to microwave vulcanization Zylox, and component and mass fraction prescription are following:
Figure FDA0000106968840000011
2. the preparation method of the Zylox of claim 1 is characterized in that sebific duct is that the speed that adopts single screw extrusion machine, cooperates microwave vulcanization to draw section carries out carrying out moulding through the mode of microwave vulcanization again after sebific duct is extruded; Concrete sulfidization molding technology controlling and process is following:
1) microwave vulcanization
Use one section microwave, three sections hot-air vulcanization equipment to carry out the microwave vulcanization moulding:
Microwave section temperature is controlled at 210 ℃～230 ℃, and one section temperature of warm air beating is 210 ℃～230 ℃, and two sections temperature of warm air beating are 210 ℃～230 ℃, and three sections temperature of warm air beating are 210 ℃～230 ℃, and pulling speed is controlled at 5～10m/min;
2) adopt the post vulcanization mode
Adopt the post cure mode of 120 ℃ * 2h after the microwave vulcanization.
CN201110353996A 2011-11-09 2011-11-09 Silicone rubber applicable to microwave curing and preparation method thereof Active CN102408725B (en)

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Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106584722A (en) * 2016-11-29 2017-04-26 际华三五五皮革皮鞋有限公司 Production process for producing rubber outsole by microwave vulcanization
CN107316675A (en) * 2017-06-22 2017-11-03 迈特诺（马鞍山）特种电缆有限公司 A kind of high iron shield power "Jumper" cable and its manufacture method
CN108342086A (en) * 2018-03-21 2018-07-31 东莞市正安有机硅科技有限公司 A kind of method of VOC in reduction silicon rubber
CN109233284A (en) * 2018-08-14 2019-01-18 天津安浩生物科技有限公司 A kind of method and device preparing bi-component copolymerized siloxanes
CN110474068A (en) * 2019-08-05 2019-11-19 上海电气集团股份有限公司 A kind of preparation method of fuel cell vulcanized sealant

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US5438081A (en) * 1994-10-20 1995-08-01 General Electric Company Microwave-activated preparation of silicone foams, and compositions useful therein
CN1746224A (en) * 2005-09-29 2006-03-15 中蓝晨光化工研究院 High and low temperature-resistant rubber with high damping
CN1769351A (en) * 2004-11-04 2006-05-10 瓦克化学有限公司 Silicone elastomer with microwave activity
CN101070430A (en) * 2007-05-16 2007-11-14 石建国 Silica-gel foaming-gel heat-insulation pipe and preparing method
CN101121820A (en) * 2007-09-19 2008-02-13 上海回天化工新材料有限公司 Halogen-free anti-flaming silicon rubber and its preparing method and use
CN101706023A (en) * 2009-12-09 2010-05-12 河北东劲液压橡塑制品有限公司 Over-pressure over-temperature environment-friendly silica gel composite pipe and preparation method thereof
CN101805520A (en) * 2010-03-19 2010-08-18 东莞市宏达新材料有限公司 Silicone self-adhesive formula and preparation method
CN102070906A (en) * 2010-12-16 2011-05-25 东莞新东方化工有限公司 Extruded silicon rubber and preparation method thereof

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JPH02261835A (en) * 1989-03-31 1990-10-24 Shin Etsu Chem Co Ltd Foamable silicone rubber composition
US5214074A (en) * 1991-01-29 1993-05-25 Shin-Etsu Chemical Co., Ltd. Foamable silicone rubber composition and silicone rubber sponge
US5438081A (en) * 1994-10-20 1995-08-01 General Electric Company Microwave-activated preparation of silicone foams, and compositions useful therein
CN1769351A (en) * 2004-11-04 2006-05-10 瓦克化学有限公司 Silicone elastomer with microwave activity
CN1746224A (en) * 2005-09-29 2006-03-15 中蓝晨光化工研究院 High and low temperature-resistant rubber with high damping
CN101070430A (en) * 2007-05-16 2007-11-14 石建国 Silica-gel foaming-gel heat-insulation pipe and preparing method
CN101121820A (en) * 2007-09-19 2008-02-13 上海回天化工新材料有限公司 Halogen-free anti-flaming silicon rubber and its preparing method and use
CN101706023A (en) * 2009-12-09 2010-05-12 河北东劲液压橡塑制品有限公司 Over-pressure over-temperature environment-friendly silica gel composite pipe and preparation method thereof
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Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106584722A (en) * 2016-11-29 2017-04-26 际华三五五皮革皮鞋有限公司 Production process for producing rubber outsole by microwave vulcanization
CN107316675A (en) * 2017-06-22 2017-11-03 迈特诺（马鞍山）特种电缆有限公司 A kind of high iron shield power "Jumper" cable and its manufacture method
CN108342086A (en) * 2018-03-21 2018-07-31 东莞市正安有机硅科技有限公司 A kind of method of VOC in reduction silicon rubber
CN108342086B (en) * 2018-03-21 2021-06-29 东莞市正安有机硅科技有限公司 Method for reducing VOC (volatile organic compounds) in silicone rubber
CN109233284A (en) * 2018-08-14 2019-01-18 天津安浩生物科技有限公司 A kind of method and device preparing bi-component copolymerized siloxanes
CN110474068A (en) * 2019-08-05 2019-11-19 上海电气集团股份有限公司 A kind of preparation method of fuel cell vulcanized sealant

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Address after: 300270 No. 1703, Ge Wan Road, Zhong Tang Industrial Zone, Binhai New Area, Tianjin

Patentee after: Tianjin Peng Ling group Limited by Share Ltd

Address before: 300384 No. 1703, Ge Wan Road, Grand Port, Tianjin

Patentee before: Tianjin Pengling Rubber Tube Co., Ltd.