CN1908067A - Preparation method of special material for injection moulding composite silicon rubber insulator mixing refine rubber - Google Patents

Preparation method of special material for injection moulding composite silicon rubber insulator mixing refine rubber Download PDF

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Publication number
CN1908067A
CN1908067A CN 200610106806 CN200610106806A CN1908067A CN 1908067 A CN1908067 A CN 1908067A CN 200610106806 CN200610106806 CN 200610106806 CN 200610106806 A CN200610106806 A CN 200610106806A CN 1908067 A CN1908067 A CN 1908067A
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Prior art keywords
parts
rubber
high temperature
agent
silicon oil
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CN 200610106806
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Chinese (zh)
Inventor
陈江明
朱德洪
祝纪才
吴国伟
何佰祥
徐连英
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JIANGSU HONGDA CHEMICAL NEW MATERIAL CO Ltd
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JIANGSU HONGDA CHEMICAL NEW MATERIAL CO Ltd
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Priority claimed from CN 200510037923 external-priority patent/CN1693368A/en
Application filed by JIANGSU HONGDA CHEMICAL NEW MATERIAL CO Ltd filed Critical JIANGSU HONGDA CHEMICAL NEW MATERIAL CO Ltd
Priority to CN 200610106806 priority Critical patent/CN1908067A/en
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Abstract

the invention discloses a preparing method of insulator melted gel, which is characterized by the following: adopting hydroxyl silicon oil through potassium hydroxide method to replace national acetic anhydride method; utilizing dynamic high-temperature method to dispose aluminium hydroxide for flame-proof material; improving mixed property and manufacturing property of gel through associating methyl phenyl hydroxyl silicon oil and silane methyl vinyl triethoxy; fitting for injecting mould.

Description

The preparation method who is used for special material for injecting forming composite silicon rubber insulator mixing refine rubber
Technical field
The present invention relates to the silicon rubber insulator technology of preparing, particularly relate to a kind of preparation method who is used for special material for injecting forming composite silicon rubber insulator mixing refine rubber with potassium hydroxide as Preparation of Catalyst.
Background technology
The composite silicone rubber insulator is the novel material that develops rapidly in recent years, and is in light weight with it, has excellent electrical insulating property and weather resistance, replaces traditional porcelain insulator just gradually.The technology of composite silicone rubber insulator employing at present is based on compression molding, and efficient is low.Injection molding composite silicone rubber insulator mainly solves the flowability of rubber unvulcanizate, can enhance productivity greatly, and Products Quality also has bigger improvement simultaneously.The hydroxy silicon oil that domestic acetic anhydride method makes, the product slant acidity when being used for rubber unvulcanizate production as antistructurizing agent, badly influences the storage period of rubber unvulcanizate, and the physical and mechanical properties after the product sulfuration is also had disadvantageous effect.
Summary of the invention
Purpose of the present invention overcomes above-mentioned deficiency exactly, effectively improves the mixed performance and the flowing property of silicon rubber, and a kind of preparation method who is used for special material for injecting forming composite silicon rubber insulator mixing refine rubber is provided.
The objective of the invention is to be achieved through the following technical solutions:
Its preparation process is:
Preparation base silicon rubber, adopting KOH is the methyl ethylene high temperature glue of Catalyst Production, molecular weight in 45~800,000 scopes, contents of ethylene 0.1~0.4%, fugitive constituent is no more than 2%.
Preparation fire-retardant filler fine aluminum hydroxide powder, wherein the aminomethyl phenyl hydroxy silicon oil is as high temperature resistant dispersion agent, the reinforcement auxiliary agent that vinyltriethoxysilane is handled as filler, treatment process is: take 100 parts in the aluminium hydroxide handled as the described dynamic high temperature of patent application 200510037924.X " a kind of aluminium hydroxide dynamic high temperature treatment process that is used for the silicon rubber flame-retardant additives agent ", 0.5~1.5 part of aminomethyl phenyl hydroxy silicon oil, 0.5~1.5 part of vinyltriethoxysilane, three kinds of raw materials are measured join in the high speed kneader, with being steam heated to 150 ℃, stir process 2 hours.
Prepare rubber unvulcanizate according to following prescription and process: 100 parts in methyl ethylene high temperature glue, releasing agent are stirred for 0.1~0.3 part in kneader, after gradation adds 25~45 parts of white carbon blacks, 5~6 parts of stirrings of antistructurizing agent hydroxy silicon oil moulding again, heat up 160~175 ℃ and fill nitrogen, vacuumize, after the discharging cooling, sizing material is cooled to room temperature, be shaped intact after, deposited 24 hours, and joined again in the kneader and to add 100~120 parts of above-mentioned fire-retardant filler fine aluminum hydroxide powders; 3 parts of red iron oxides; 0.4 part of vulcanizing agent, roller, thin-pass, filter glue, packing are wrapped in the mixing moulding discharging then.
Advantage of the present invention:
(1) hydroxy silicon oil that adopts the hydroxy silicon oil of potassium hydroxide method production to replace domestic acetic anhydride method to make, it is neutral that product is, when being used for rubber unvulcanizate production as antistructurizing agent, greatly prolonged the storage period of rubber unvulcanizate, extending near half a year during by the hydroxy silicon oil that adopts domestic acetic anhydride method to make less than one month.Simultaneously the physical and mechanical properties after the product sulfuration is also increased.
(2) adopt through taking of handling of dynamic high temperature and do fire-retardant filler, can improve its dispersing uniformity in mixing process as the fine aluminum hydroxide powder that the described dynamic high temperature of patent application 200510037924.X " a kind of aluminium hydroxide dynamic high temperature treatment process that is used for the silicon rubber flame-retardant additives agent " is handled.
(3) adopt above-mentioned dynamic high temperature method to handle fine aluminum hydroxide powder,, can improve the mixed performance and the flowing property of rubber unvulcanizate by forming fire-retardant filler with aminomethyl phenyl hydroxy silicon oil and methyl ethylene triethoxyl silane associated treatment.
(4) special material for injecting forming composite silicon rubber insulator mixing refine rubber of the inventive method preparation can be applicable to injection molding production, has solved the high temperature injection flowability of rubber unvulcanizate.
The special material for injecting forming composite silicon rubber insulator mixing refine rubber physical and mechanical properties of the inventive method preparation is as follows: hardness (Shao A) 59~62; Tensile strength 6.20~8.87Mpa; Elongation 320~350%; Tearing toughness 16.2~20.5Kn/m; Plasticity number 213~244%; Compression set is less than 2%; Rebound resilience 50~55%.
The electrical insulation capability index is as follows: surface resistivity (2.85~3.66) * 1013 Ω cm; Volume specific resistance (1.44~1.93) * 1013 Ω cm; Power frequency DIELECTRIC CONSTANT 3.85~4.63; Dielectric loss angle tangent (1.89~2.23) * 10-2; Power frequency punctures dielectric strength (19.25~23.17) kV/mm; Flammability test meets FVO grade standard value regulation, reaches qualified.The test of creepage trace and galvanic corrosion damage property meets 1A4.5 grade standard value regulation, reaches qualified.
Description of drawings
Fig. 1 technical process schematic block diagram
Embodiment
Embodiment 1:
Adopting KOH is the methyl ethylene high temperature glue of catalyzer through vacuum hydro-extraction and second dehydration explained hereafter, preparation base silicon rubber.
Preparation fire-retardant filler fine aluminum hydroxide powder, wherein the aminomethyl phenyl hydroxy silicon oil is as high temperature resistant dispersion agent, the reinforcement auxiliary agent that vinyltriethoxysilane is handled as filler, treatment process is: 100 parts in aluminium hydroxide, 0.5~1.5 part of aminomethyl phenyl hydroxy silicon oil, 0.5~1.5 part of vinyltriethoxysilane measures three kinds of raw materials and joins in the high speed kneader, with being steam heated to 150 ℃, stir process 2 hours.
According to following prescription: 100 parts in methyl ethylene high temperature glue; 25 parts of white carbon blacks; 5 parts of antistructurizing agent hydroxy silicon oils; 0.1 part of releasing agent; 120 parts in aluminium hydroxide; 3 parts of red iron oxides; 0.4 part of vulcanizing agent.In the 500L kneader, add double centner methyl ethylene high temperature glue and 0.1 kilogram of releasing agent, after start stirs, divide three times and add 25 kilograms of thermal silicas, add 15 kilograms, 10 kilograms, 10 respectively in gram at every turn, be as the criterion through stir preliminary moulding with sizing material pitch time.Add 5 kilograms of antistructurizing agent hydroxy silicon oils simultaneously, after the stirring moulding, be warming up to 160 ℃ and handled 1 hour, vacuumized the discharging cooling again 0.5 hour.The sizing material cooling is put into the treated auxiliary agents such as aluminium hydroxide of adding in the kneader after 24 hours again, and the mixing moulding discharging through bag roller, filtration, packing, obtains 252.8 kilograms of special material for injecting forming composite silicon rubber insulator mixing refine rubber.Measuring its physical and mechanical properties through the sulfuration test piece is: hardness (Shao A) 61; Tensile strength 6.20Mpa; Elongation 320%; Tearing toughness 16.2Kn/m; Plasticity number 213%; Compression set 1.87%; Rebound resilience 54%.Electrical insulation capability: surface resistivity 3.24 * 1013 Ω cm; Volume specific resistance 1.64 * 1013 Ω cm; Power frequency DIELECTRIC CONSTANT 4.29; Dielectric loss angle tangent 2.01 * 10-2; Power frequency punctures dielectric strength 21.69kV/mm; Flammability test meets FVO grade standard value regulation, and is qualified.The test of creepage trace and galvanic corrosion damage property meets 1A4.5 grade standard value regulation, and is qualified.
Embodiment 2:
With embodiment 1 preparation base silicon rubber, fire-retardant filler fine aluminum hydroxide powder, again according to following prescription, 100 parts in methyl ethylene high temperature glue; 40 parts of white carbon blacks; 6 parts of antistructurizing agent hydroxy silicon oils; 0.2 part of releasing agent; 110 parts in aluminium hydroxide; 3 parts of red iron oxides; Vulcanizing agent adds double centner methyl ethylene high temperature glue and 0.2 kilogram of releasing agent for 0.4 part in the 500L kneader, after start stirs, divide secondary to add 40 kilograms of thermal silicas, add 25 kilograms, 15 kilograms at every turn respectively, be as the criterion through stir preliminary moulding with sizing material pitch time.Add 6 kilograms of antistructurizing agent hydroxy silicon oils simultaneously, after the stirring moulding, be warming up to 170 ℃ and handled 1 hour, vacuumized the discharging cooling again 0.5 hour.The sizing material cooling is put into the treated auxiliary agents such as aluminium hydroxide of adding in the kneader after 24 hours again, and the mixing moulding discharging through bag roller, filtration, packing, obtains 258.4 kilograms of special material for injecting forming composite silicon rubber insulator mixing refine rubber.Measuring its physical and mechanical properties through the sulfuration test piece is: hardness (Shao A) 59; Tensile strength 7.30Mpa; Elongation 333%; Tearing toughness 19.5Kn/m; Plasticity number 231%; Compression set 1.79%; Rebound resilience 53%.Electrical insulation capability: surface resistivity 3.44 * 1013 Ω cm; Volume specific resistance 1.75 * 1013 Ω cm; Power frequency DIELECTRIC CONSTANT 4.55; Dielectric loss angle tangent 2.31 * 10-2; Power frequency punctures dielectric strength 22.77kV/mm; Flammability test meets FVO grade standard value regulation, and is qualified.The test of creepage trace and galvanic corrosion damage property meets 1A4.5 grade standard value regulation, and is qualified.
Embodiment 3:
With embodiment 1 preparation base silicon rubber, fire-retardant filler fine aluminum hydroxide powder, again according to following prescription, 100 parts in methyl ethylene high temperature glue; 35 parts of white carbon blacks; 6 parts of antistructurizing agent hydroxy silicon oils; 0.3 part of releasing agent; 115 parts in aluminium hydroxide; 3 parts of red iron oxides; 0.4 part of vulcanizing agent.In the 500L kneader, add double centner methyl ethylene high temperature glue and 0.3 kilogram of releasing agent, after start stirs, divide three times and add 35 kilograms of thermal silicas, add 20 kilograms, 10 kilograms, 10 kilograms at every turn respectively, be as the criterion through stir preliminary moulding with sizing material pitch time.Add 6 kilograms of antistructurizing agent hydroxy silicon oils simultaneously, after the stirring moulding, be warming up to 165 ℃ and handled 1 hour, vacuumized the discharging cooling again 0.5 hour.The sizing material cooling is put into the treated auxiliary agents such as aluminium hydroxide of adding in the kneader after 24 hours again, and the mixing moulding discharging through bag roller, filtration, packing, obtains 258.3 kilograms of special material for injecting forming composite silicon rubber insulator mixing refine rubber.Measuring its physical and mechanical properties through the sulfuration test piece is: hardness (Shao A) 60; Tensile strength 8.22Mpa; Elongation 335%; Tearing toughness 19.7Kn/m; Plasticity number 226%; Compression set 1.89%; Rebound resilience 52%.Electrical insulation capability: surface resistivity 3.78 * 1013 Ω cm; Volume specific resistance 1.62 * 1013 Ω cm; Power frequency DIELECTRIC CONSTANT 4.58; Dielectric loss angle tangent 2.44 * 10-2; Power frequency punctures dielectric strength 23.07kV/mm; Flammability test meets FVO grade standard value regulation, and is qualified.The test of creepage trace and galvanic corrosion damage property meets 1A4.5 grade standard value regulation, and is qualified.

Claims (1)

1. the preparation method who is used for special material for injecting forming composite silicon rubber insulator mixing refine rubber, it is characterized in that for:
A. prepare base silicon rubber, adopting KOH is the methyl ethylene high temperature glue of Catalyst Production, its molecular weight in 45~800,000 scopes, contents of ethylene 0.1~0.4%, fugitive constituent is no more than 2%;
B. prepare the fire-retardant filler fine aluminum hydroxide powder, wherein the aminomethyl phenyl hydroxy silicon oil is as high temperature resistant dispersion agent, the reinforcement auxiliary agent that vinyltriethoxysilane is handled as filler, treatment process is: 100 parts in the aluminium hydroxide that the process dynamic high temperature is handled, 0.5~1.5 part of aminomethyl phenyl hydroxy silicon oil, 0.5~1.5 part of vinyltriethoxysilane measures three kinds of raw materials and joins in the high speed kneader, with being steam heated to 150 ℃, stir process 2 hours;
C. prepare rubber unvulcanizate according to following prescription and process: 100 parts in methyl ethylene high temperature glue, releasing agent are stirred for 0.1~0.3 part in kneader, after gradation adds 25~35 parts of white carbon blacks, 5~6 parts of stirrings of antistructurizing agent hydroxy silicon oil moulding again, heat up 160~175 ℃ and fill nitrogen, vacuumize, after the discharging cooling, sizing material is cooled to room temperature, be shaped intact after, deposited 24 hours, and joined in the kneader again, and add 100~120 parts of above-mentioned fire-retardant filler fine aluminum hydroxide powders; 3 parts of red iron oxides; 0.4 part of vulcanizing agent, roller, thin-pass, filter glue, packing are wrapped in the mixing moulding discharging then.
CN 200610106806 2005-07-21 2006-07-21 Preparation method of special material for injection moulding composite silicon rubber insulator mixing refine rubber Pending CN1908067A (en)

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CN200510037923.5 2005-07-21
CN 200510037923 CN1693368A (en) 2005-07-21 2005-07-21 Process for preparing special material for injecting forming composite silicon rubber insulator mixing refine rubber
CN 200610106806 CN1908067A (en) 2005-07-21 2006-07-21 Preparation method of special material for injection moulding composite silicon rubber insulator mixing refine rubber

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Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101840758A (en) * 2010-05-27 2010-09-22 苏州英丝雷帝电气有限公司 Production process of composite insulator by integral injection molding without positioning device
CN102585513A (en) * 2011-12-31 2012-07-18 全超 Silicone rubber insulation material applied to high voltage cable accessories in European series and preparation method for material
CN105038255A (en) * 2015-07-06 2015-11-11 安徽创宇电力设备有限公司 Heatproof composite insulator
CN105175787A (en) * 2015-07-21 2015-12-23 山东晨旭新材料股份有限公司 Preparation method for composite insulator used active aluminum hydroxide

Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101840758A (en) * 2010-05-27 2010-09-22 苏州英丝雷帝电气有限公司 Production process of composite insulator by integral injection molding without positioning device
CN102585513A (en) * 2011-12-31 2012-07-18 全超 Silicone rubber insulation material applied to high voltage cable accessories in European series and preparation method for material
CN102585513B (en) * 2011-12-31 2015-08-12 全超 A kind ofly be applied to silicon rubber insulation sizing material of European serial medium and high voltage cable annex and preparation method thereof
CN105038255A (en) * 2015-07-06 2015-11-11 安徽创宇电力设备有限公司 Heatproof composite insulator
CN105175787A (en) * 2015-07-21 2015-12-23 山东晨旭新材料股份有限公司 Preparation method for composite insulator used active aluminum hydroxide

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