CN108513380A - Solvent-less organosilicon resin coating heating element insulation filling material production method - Google Patents

Solvent-less organosilicon resin coating heating element insulation filling material production method Download PDF

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Publication number
CN108513380A
CN108513380A CN201810009897.2A CN201810009897A CN108513380A CN 108513380 A CN108513380 A CN 108513380A CN 201810009897 A CN201810009897 A CN 201810009897A CN 108513380 A CN108513380 A CN 108513380A
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China
Prior art keywords
resin coating
organic
heating element
filling material
solvent
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CN201810009897.2A
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Chinese (zh)
Inventor
庄伟兵
宗俊
金宏伟
刘荣栋
潘文斌
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SHANGHAI INDUSTRIAL ZHENTAI CHEMICAL INDUSTRIAL Co Ltd
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SHANGHAI INDUSTRIAL ZHENTAI CHEMICAL INDUSTRIAL Co Ltd
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Priority to CN201810009897.2A priority Critical patent/CN108513380A/en
Publication of CN108513380A publication Critical patent/CN108513380A/en
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    • HELECTRICITY
    • H05ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
    • H05BELECTRIC HEATING; ELECTRIC LIGHT SOURCES NOT OTHERWISE PROVIDED FOR; CIRCUIT ARRANGEMENTS FOR ELECTRIC LIGHT SOURCES, IN GENERAL
    • H05B3/00Ohmic-resistance heating
    • H05B3/40Heating elements having the shape of rods or tubes
    • H05B3/42Heating elements having the shape of rods or tubes non-flexible
    • H05B3/48Heating elements having the shape of rods or tubes non-flexible heating conductor embedded in insulating material
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01BCABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
    • H01B3/00Insulators or insulating bodies characterised by the insulating materials; Selection of materials for their insulating or dielectric properties
    • H01B3/02Insulators or insulating bodies characterised by the insulating materials; Selection of materials for their insulating or dielectric properties mainly consisting of inorganic substances
    • H01B3/10Insulators or insulating bodies characterised by the insulating materials; Selection of materials for their insulating or dielectric properties mainly consisting of inorganic substances metallic oxides
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01BCABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
    • H01B3/00Insulators or insulating bodies characterised by the insulating materials; Selection of materials for their insulating or dielectric properties
    • H01B3/18Insulators or insulating bodies characterised by the insulating materials; Selection of materials for their insulating or dielectric properties mainly consisting of organic substances
    • H01B3/30Insulators or insulating bodies characterised by the insulating materials; Selection of materials for their insulating or dielectric properties mainly consisting of organic substances plastics; resins; waxes
    • H01B3/46Insulators or insulating bodies characterised by the insulating materials; Selection of materials for their insulating or dielectric properties mainly consisting of organic substances plastics; resins; waxes silicones
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01BCABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
    • H01B3/00Insulators or insulating bodies characterised by the insulating materials; Selection of materials for their insulating or dielectric properties
    • H01B3/18Insulators or insulating bodies characterised by the insulating materials; Selection of materials for their insulating or dielectric properties mainly consisting of organic substances
    • H01B3/30Insulators or insulating bodies characterised by the insulating materials; Selection of materials for their insulating or dielectric properties mainly consisting of organic substances plastics; resins; waxes
    • H01B3/46Insulators or insulating bodies characterised by the insulating materials; Selection of materials for their insulating or dielectric properties mainly consisting of organic substances plastics; resins; waxes silicones
    • H01B3/465Silicone oils

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  • Chemical & Material Sciences (AREA)
  • Physics & Mathematics (AREA)
  • Spectroscopy & Molecular Physics (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Engineering & Computer Science (AREA)
  • Ceramic Engineering (AREA)
  • Inorganic Chemistry (AREA)
  • Paints Or Removers (AREA)
  • Organic Insulating Materials (AREA)
  • Resistance Heating (AREA)

Abstract

The present invention proposes a kind of production method of heating element insulation filling material, includes the following steps:Highly viscous organic siliconresin is uniformly mixed with the organic silicone oil of low viscosity, forms silicone fluid;Step mixed uniformly silicone fluid diaphragm pump is sprayed into operation;Silicone fluid is wrapped in mgo surface by the mechanical equipment of action of forced stirring;By the magnesia powder of step silicone resin coating at a temperature of 200~300 DEG C baking and curing so that oxidation powder have good fluidity, be easy to the magnesia powder filling operation of electrothermal tube.By the magnesia powder natural cooling of step silicone resin coating, final products are obtained by the sieve of 0.425mm.This method uses the composite organic material of organic oil without using organic solvent, magnesia powder manufacturing cost is set to be declined, environment hidden danger is thoroughly solved, and is all suitable for the magnesia powder of all silicone resin coatings, and can achieve the purpose that preferable insulation performance in the case where amount is few.

Description

Solvent-less organosilicon resin coating heating element insulation filling material production method
Technical field
The present invention relates to a kind of production method of tubular electrothermal element insulation filling material, more particularly to one kind are solvent-free Silicone resin coating heating element insulation filling material production method.
Background technology
Tubular electrothermal element (abbreviation electrothermal tube) is usually made of three parts:Metal shell, heating wire and insulation filling material Material.The effects that wherein insulation filling material plays fixed heating wire, transmits heat and provide enough electrical insulation capabilities.Due to Electrically molten magnesia has good thermal conductivity and high temperature electrical insulating property, thus is widely used as the insulation filling material of electrothermal tube Material.After electrothermal tube filling, after the processes such as the draw, usually there are two types of the modes of operation before molding procedure, first, without overheat Direct brake forming is handled, second is that needing the brake forming after the heat treatment of the softening tubing of certain temperature environment.Wherein The mode of 2 points of heat treatments is subdivided into two kinds of processing modes of low temperature and high temperature.Low Temperature Heat Treatment typically refers to heat treatment temperature and exists 200~650 DEG C of ranges, for the equipment used based on baking oven and tunnel stove, the object of processing is iron pipe, aluminum pipe, copper pipe and part Stainless steel tube material.High-temperature heat treatment typically refers to heat treatment temperature in 1050~1100 DEG C of ranges, and the equipment used is tunnel The object of stove, processing is stainless steel pipe material (playing emollescence, eliminate the part stress of material).
In order to control minimum manufacturing cost, the product of electrothermal tube total amount 60~70% in the market at present is all before molding Using Low Temperature Heat Treatment or by the way of need not being heat-treated.Also to insulation filling material, (fused magnesium oxide powder is commonly called as oxygen simultaneously Change magnesium powder or magnesium powder) propose very high requirement, it needs to remain to keep qualified insulation performance under such heat treatment condition.
In order to obtain suitable processing performance (fill insulant when tubular electrothermal element is processed), usually by blocky electric smelting Magnesia powder is broken into graininess powder of the grain size between 0.425mm~0.045mm, and adjusts the percentage of each grain size as required To obtain suitable tap density and mobility.
However pure electrically molten magnesia generally cannot be directly as packing material, this is because pure electric smelting oxygen magnesium has hydrophilic spy Property, do not have the insulation performance of hydrophobic.Specific manifestation be by the cold insulation resistance rate of its tubular electrothermal element obtained it is relatively low, And even insulation is zero after declining several hours always.Especially relative air humidity RH values are more than 80% climatic environment Under, in 30 minutes the insulation of heating element just drop to zero.
These electrothermal tubes propose the insulation performance of used magnesia powder harsh requirement, silicone resin material The low-temperature oxidation magnesium powder of coating disclosure satisfy that above-mentioned requirements, can not only bear Low Temperature Heat Treatment and be wanted to the heatproof of organosilicon material It asks, also disclosure satisfy that the insulating requirements of electrothermal tube.
A kind of common method is that some silicone resin materials are added in magnesia, so as to improve the electrical isolation of electrothermal tube Performance.The method being commonly used is:Machine silicones is wrapped in the surface of magnesia particle with certain content, is formed organic The coating of silicones completely cuts off the intrusion of moisture.
However this method there are problems that, be embodied in:
1, in order to make coating operation smoothly implement, the viscosity of organosilicon material must control 1000 (cp.25 DEG C) with Under, due to the limitation of viscosity, the organosilicon material silicones in this kind of insulating materials has to use organic solvent (ethyl alcohol, toluene Or styrene etc.) coating operation that can be smoothed out is diluted, obtain the effect of preferable coated powder particle;
2, secondly the use recycling of organic solvent not only increases manufacturing cost, and to environment also larger pollution hidden trouble.
So a kind of organic solvent diluting that can not use of invention can carry out the organosilicon tree of magnesia powder coating operation Fat production method becomes particularly significant.
Invention content
The object of the present invention is to provide a kind of solvent-less organosilicon resin coating heating elements to be made of insulation filling material Method, to overcome drawbacks described above.
The present invention be solve its technical problem the technical scheme adopted is that
Solvent-less organosilicon resin coating heating element insulation filling material production method, includes the following steps:
(1) highly viscous organic siliconresin is uniformly mixed with the organic silicone oil of low viscosity, forms silicone fluid;
(2) diaphragm pump of mixed uniformly silicone fluid in step (1) is sprayed into operation;
(3) silicone fluid is wrapped in by the mechanical equipment of action of forced stirring by mgo surface;
(4) magnesia powder for the silicone resin coating that step (3) is formed is dried at a temperature of 200~300 DEG C solid Change so that oxidation powder has good fluidity, is easy to the magnesia powder filling operation of electrothermal tube.
(5) it by the magnesia powder natural cooling of step (4) silicone resin coating, is obtained most by the sieve of 0.425mm Finished product.
In step (1), the viscosity of silicone fluid is controlled at 500cp.25 DEG C hereinafter, being easy to spray operation.
In step (1), organic siliconresin and organic silicone oil are 2 kinds in poly- methylsiloxane oxygen alkane or organosiloxane Or two or more, the mass ratio of organic siliconresin and organic silicone oil is 1:3~1:5;The viscosity of organic siliconresin be 2000~ 4000cp.25 DEG C, the viscosity of organic silicone oil is 10~30cp.25 DEG C.
In step (1), liquid mixing time is 0.2h~0.5h.
In step (2), diaphragm pump is pneumatic equipment, and outlet pressure is more than 6kgf/cm3, it is below 10000cp can be conveyed Liquid.
In step (3), it is to be proportionally added into organic silicon solution that organic silicon solution, which is wrapped in electrically molten magnesia surface, In granular magnesia, and implemented by blender stirring, mixing time is 30~180 minutes.
In step (3), the mass ratio between silicone fluid and magnesia is 1:300-1:1000.
In step (4), hardening time is 0.25h~1h.
The advantage of the invention is that:
The use of this method organic siliconresin meets electrothermal tube under the heat treatment condition of 200~650 DEG C of ranges, remains to Good insulation performance is kept, without using organic solvent using the composite organic material of organic oil, magnesia powder is made to manufacture Cost is declined, and environment hidden danger is thoroughly solved, and is all suitable for the magnesia powder of all silicone resin coatings, and can To achieve the purpose that preferable insulation performance in the case where amount is few.
Specific implementation mode
In order to make the technical means, the creative features, the aims and the efficiencies achieved by the present invention be easy to understand, tie below Specific embodiment is closed, the present invention is further explained.
Embodiment:
1, blocky electrically molten magnesia emery dust is broken into graininess powder of the grain size between 0.425mm~0.045mm, and pressed It is required that magnesia powder obtained by each grain size percentage of adjustment.
2, it is in mass ratio 1 by the organic silicone oil of highly viscous organic siliconresin and low viscosity:3 15~20 points of stirrings Clock makes liquid uniformly mix, and it is 630cp.25 DEG C (with reference to ASTM D445 standard methods) to measure viscosity.
3, the magnesia 4000Kg with appropriate grain size proportion is poured into mixing plant, uniformly having for step 2 preparation is added Machine silicon liquid 10Kg, mass ratio 1:400 stirrings 60 minutes;
4, baking and curing 1.5h at a temperature of 25~280 DEG C;
5, cooling in spontaneously drying environment;
7, it is sieved and packs:25Kg/ casees.
Into the water by product obtained, magnesia powder shows hydrophobic tight agglomeration in water.Test is made Reach 200~600M Ω with 6 measurement insulation performances of standard electrothermal tube, through 200 DEG C, 450 DEG C, multiple temperature conditions such as 650 DEG C Under heat treatment, measure electrothermal tube insulation performance reach 100,000~1,000,000 M Ω.The above experimental result explanation is without organic siliconresin The performance of the magnesia powder of coating is qualified, and the requirement that can meet making tubulose electrothermal tube insulation performance is (general to require greatly In 1000M Ω).In order to compare, we test the product (silicone resin material of conventional method manufacture using same method With toluene in mass ratio 1:5 dilutions) and pure magnesia insulation performance (unit M Ω) in the same state, test result is shown in Table 1.
The insulation resistance of 1 each packing material of table and performance of swimming
Note:Insulation Resistance Tester device is:SUPER MEGOHMMETER SM-8215 types (Japanese TOA&DKK companies)
It can see from the result in table 1, method either provided by the invention or traditional method can meet electricity Insulation performance of the heat pipe to magnesia powder.It is just obtained and tradition side as diluent however, the present invention does not need organic solvent The identical effect of method.
Illustrate the insulating properties of the solvent-less organosilicon resin coating heating element insulation filling material prepared with the present invention Can, comply fully with the demand in market in the condition of Low Temperature Heat Treatment.
Embodiment of above only technical concepts and features to illustrate the invention, its object is to allow those skilled in the art Member understands present disclosure and is implemented, and it is not intended to limit the scope of the present invention, all according to spirit of that invention The equivalent change or modification that essence is done should all cover within the scope of the present invention.

Claims (8)

1. solvent-less organosilicon resin coating heating element insulation filling material production method, which is characterized in that including following Step:
(1) highly viscous organic siliconresin is uniformly mixed with the organic silicone oil of low viscosity, forms silicone fluid;
(2) diaphragm pump of mixed uniformly silicone fluid in step (1) is sprayed into operation;
(3) silicone fluid is wrapped in by the mechanical equipment of action of forced stirring by mgo surface;
(4) magnesia powder for the silicone resin coating for forming step (3) baking and curing at a temperature of 200~300 DEG C;
(5) it by the magnesia powder natural cooling of step (4) silicone resin coating, is finally produced by the sieve of 0.425mm Product.
2. solvent-less organosilicon resin coating heating element insulation filling material production method according to claim 1, It is characterized in that:
In step (1), the viscosity of silicone fluid is controlled at 500cp.25 DEG C or less.
3. solvent-less organosilicon resin coating heating element insulation filling material production method according to claim 1, It is characterized in that:
In step (1), organic siliconresin and organic silicone oil are 2 kinds or 2 in poly- methylsiloxane oxygen alkane or organosiloxane Kind or more, the mass ratio of organic siliconresin and organic silicone oil is 1:3~1:5;The viscosity of organic siliconresin be 2000~ 4000cp.25 DEG C, the viscosity of organic silicone oil is 10~30cp.25 DEG C.
4. solvent-less organosilicon resin coating heating element insulation filling material production method according to claim 1, It is characterized in that:
In step (1), liquid mixing time is 0.2h~0.5h.
5. solvent-less organosilicon resin coating heating element insulation filling material production method according to claim 1, It is characterized in that:
In step (2), diaphragm pump is pneumatic equipment, and outlet pressure is more than 6kgf/cm3, 10000cp liquid below can be conveyed.
6. solvent-less organosilicon resin coating heating element insulation filling material production method according to claim 1, It is characterized in that:
In step (3), it is that organic silicon solution is proportionally added into graininess that organic silicon solution, which is wrapped in electrically molten magnesia surface, Magnesia in, and by blender stirring implement, mixing time be 30~180 minutes.
7. solvent-less organosilicon resin coating heating element insulation filling material production method according to claim 1, It is characterized in that:
In step (3), the mass ratio between silicone fluid and magnesia is 1:300-1:1000.
8. solvent-less organosilicon resin coating heating element insulation filling material production method according to claim 1, It is characterized in that:
In step (4), hardening time is 0.25h~1h.
CN201810009897.2A 2018-01-05 2018-01-05 Solvent-less organosilicon resin coating heating element insulation filling material production method Pending CN108513380A (en)

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Application Number Priority Date Filing Date Title
CN201810009897.2A CN108513380A (en) 2018-01-05 2018-01-05 Solvent-less organosilicon resin coating heating element insulation filling material production method

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Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101688060A (en) * 2007-06-22 2010-03-31 金伯利-克拉克环球有限公司 multifunctional silicone blends
CN102220010A (en) * 2011-05-27 2011-10-19 黄山市强路新材料有限公司 Solvent-free addition liquid state silicon resin and preparation method of solvent-free addition liquid state silicon resin
CN102276987A (en) * 2011-05-27 2011-12-14 黄山市强路新材料有限公司 Solvent-free addition type liquid silicon resin
CN103442465A (en) * 2013-05-31 2013-12-11 镇江天信电器有限公司 Electric heating pipe
CN103971786A (en) * 2013-12-27 2014-08-06 上海实业振泰化工有限公司 Electric-grade organic coating high-temperature-resistant insulating magnesia powder for electric ovens and production method of electric-grade organic coating high-temperature-resistant insulating magnesia powder
CN105219100A (en) * 2015-11-12 2016-01-06 三友(天津)高分子技术有限公司 A kind of organic silicon resin encapsulant for LED and preparation method thereof

Patent Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101688060A (en) * 2007-06-22 2010-03-31 金伯利-克拉克环球有限公司 multifunctional silicone blends
CN102220010A (en) * 2011-05-27 2011-10-19 黄山市强路新材料有限公司 Solvent-free addition liquid state silicon resin and preparation method of solvent-free addition liquid state silicon resin
CN102276987A (en) * 2011-05-27 2011-12-14 黄山市强路新材料有限公司 Solvent-free addition type liquid silicon resin
CN103442465A (en) * 2013-05-31 2013-12-11 镇江天信电器有限公司 Electric heating pipe
CN103971786A (en) * 2013-12-27 2014-08-06 上海实业振泰化工有限公司 Electric-grade organic coating high-temperature-resistant insulating magnesia powder for electric ovens and production method of electric-grade organic coating high-temperature-resistant insulating magnesia powder
CN105219100A (en) * 2015-11-12 2016-01-06 三友(天津)高分子技术有限公司 A kind of organic silicon resin encapsulant for LED and preparation method thereof

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Application publication date: 20180907