CN1117699C - Preparation of high temperature resisting electrothermal insulating magnesia material - Google Patents
Preparation of high temperature resisting electrothermal insulating magnesia material Download PDFInfo
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- CN1117699C CN1117699C CN 00130288 CN00130288A CN1117699C CN 1117699 C CN1117699 C CN 1117699C CN 00130288 CN00130288 CN 00130288 CN 00130288 A CN00130288 A CN 00130288A CN 1117699 C CN1117699 C CN 1117699C
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- tetraethyl silicate
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Abstract
The present invention relates to a preparation method for high temperature resistance electrothermal insulation magnesia materials. Firstly, anhydrous alcohol is added to a container which is filled with ethyl silicate, the other anhydrous alcohol is taken and mixed with distilled water and phosphoric acid, a mixed solution is obtained, the mixed solution is slowly added into the container which is filled with ethyl silicate, stirred and stood, and SiO2 colloidal sol is formed. Magnesium oxide powder materials are added to the colloidal sol, a mixture which is obtained is uniformly stirred, dried, calcined and ground, and the electrothermal insulation materials of the present invention are obtained. In the method of the present invention, the SiO2 is uniformly coated on the surface of the magnesium oxide powder materials or uniformly dispersed in the magnesium oxide powder materials so as to obviously enhance the electrothermal insulation performance of the magnesium oxide powder materials at the high temperature.
Description
The present invention relates to a kind of preparation method of high temperature resisting electrothermal insulating magnesia material, belong to electrical insulating material technical field.
Along with the development of household electric appliances, the demand of all kinds of electric insulating materials is increasing, and according to preliminary market survey, the annual demand in the whole nation is approximately several ten thousand to tens0000 tons.Electrothermal tube is filled the insulating material of usefulness, main at present electrically molten magnesia (MgO) powder that uses.Electrical isolation MgO powder mainly is divided into low temperature modification (below 500 ℃), middle warm type (below 800 ℃) and high temperature modification (below 1200 ℃) three major types both at home and abroad at present.At present the demand major part of domestic manufacturer will be leaned on import, and especially the high temperature resistant type magnesia powder is domestic does not also have a sophisticated manufacturing technology.
In order to adapt to the requirement of electrothermal tube with insulating material, from the beginning of the nineties, domesticly just begin to solve the modification problem of electric smelting MgO powder, the main silicone covering treatment technology that adopts, solved at present the moistureproof problem of low temperature of electric smelting MgO substantially, and in, the electrical performance issues of the electrical isolation MgO powder that uses under the low temperature.Since nearly ten years, the electrical performance issues of modification MgO under the condition of high temperature is based on by more domestic R﹠D institutions and manufacturing enterprise.And adopt present silicone covering treatment technology, can't realize the use at high temperature of MgO powder, because through the MgO of silicone covering powder after the pyroprocessing more than 900 ℃, organosilicon decomposes, cause the reduction of MgO electrical insulation capability, thereby cause electrothermal component can't use (decreasing insulating and leakage current are excessive), this is the insurmountable subject matter of domestic electrothermal tube manufacturer always.For example, application number is 96120443.5, name is called the patent application of " a kind of magnesium oxide powder and manufacture method thereof with the silicone resin modification ", a kind of employing silicone resin modified magnesium powder end is disclosed, improve the technology that it loads process flowability and hydrophobic nature, but because the silicone resin non-refractory, the magnesium oxide powder of Zhi Zaoing is unfavorable at high temperature using in this way.
One of gordian technique of electrothermal tube components and parts is to use suitable electrical isolation protecting materials, and according to the retrieval, China does not also have the manufacturing technology of high temperature oxidation resisting magnesium powder electric insulating material at present.
The objective of the invention is to propose a kind of preparation method of high temperature resisting electrothermal insulating magnesia material, adopt treatment technologies such as sol-gel, electric smelting MgO powder is carried out coated Si O
2Handle Deng modification, the electrical isolation stopping composition when at high temperature using to improve MgO powder electrical insulation capability at high temperature, to make it to be suitable for electrothermal tube uses.
The preparation method of the high temperature resisting electrothermal insulating magnesia material that the present invention proposes may further comprise the steps:
(1). dehydrated alcohol is joined in the container of placing tetraethyl silicate, stirred 0.5 hour, wherein, the alcoholic acid add-on is: tetraethyl silicate: (tetraethyl silicate+2 * ethanol)=0.1～0.3: 1, tetraethyl silicate and ethanol are volume unit;
(2). other gets dehydrated alcohol a and (1) step equal volume, is mixed into mixing solutions with distilled water, phosphoric acid, and wherein, the add-on of distilled water is in molar ratio: water: tetraethyl silicate=1～5: 1 calculates; The add-on of phosphoric acid is in molar ratio: phosphoric acid: tetraethyl silicate=0.01～0.1: 1 calculates;
(3). the mixing solutions in (2) step is slowly joined under whipped state in the container in (1) step, stirred simultaneously 1 hour, container is built, left standstill 24 hours, promptly form SiO
2Colloidal sol, stand-by;
(4). with above-mentioned SiO
2Colloidal sol stirs, slowly add simultaneously the MgO powder after deironing and drying treatment, stir, the add-on of MgO powder is: MgO=(5.38～53.8) * tetraethyl silicate * tetraethyl silicate proportion, wherein tetraethyl silicate is volume unit, and MgO is a mass unit;
(5). the material in (4) is dry under whipped state, treat that liquid disappears after, stop to stir, 80 ℃ of oven dry 24 hours in baking oven then make the material thorough drying;
(6). the material in (5) is put into alumina crucible, calcine in air atmosphere, calcining temperature is 600～1000 ℃, is incubated 1～6 hour, and after cooling was come out of the stove, vibration mill 6 hours was the high temperature resisting electrothermal insulating magnesia material that the present invention prepares.
Use method of the present invention, can be with SiO
2Be coated in equably the MgO powder the surface or be evenly dispersed in the MgO powder, thereby improve MgO powder electrical insulation capability at high temperature significantly.MgO powder after the present invention handles has following electrical insulation capability:
1). as packing material, the electrothermal tube of making is after integrally annealed in 1050 ℃, 30 minutes with the MgO powder of the present invention preparation, and electrical property reaches:
Surface load 6W/cm
2The time, leakage current is less than 0.010mA (switching on 20 minutes)
Surface load 8W/cm
2The time, leakage current is less than 0.040mA (switching on 20 minutes)
2). flow velocity: φ 4m/m aperture under meter, the time is less than 40s/100g
3). compacted density: reach 2～2.38g/cm
3
Above electrical insulation capability has reached the service requirements of high temperature MgO electrically insulating material.
Introduce embodiments of the invention below.
Embodiment one:
(1). get tetraethyl silicate 100ml and put into container, under whipped state, add the 450ml dehydrated alcohol, and stirred 0.5 hour.
(2). other gets a 450ml dehydrated alcohol, is mixed into mixing solutions with 16g distilled water, 2.2g phosphoric acid.
(3). the mixing solutions in (2) step is slowly joined under whipped state in the container in (1) step, stirred simultaneously 1 hour.
(4). container is built, left standstill 24 hours, promptly form SiO
2Colloidal sol, stand-by.
(5). with above-mentioned SiO
2Colloidal sol stirs, and slowly adds the MgO powder after deironing and drying treatment simultaneously, stirs.Wherein, the add-on of MgO powder is 2690g.
(6). the material in (5) is dry under whipped state, treat that liquid disappears after, stop to stir.Then in baking oven 80 ℃ the oven dry 24 hours, make the material thorough drying.
(7). the material in (6) is put into alumina crucible, calcine in air atmosphere, calcining temperature is 650 ℃, is incubated 4 hours.
(8). cooled material in (7) is come out of the stove, and vibration mill 6 hours is the high temperature resisting electrothermal insulating magnesia material that the present invention prepares.
(9). the tubulature test:
MgO powder after the above-mentioned processing is packed in the electrothermal tube of test, and then 1000 ℃ of integrally annealeds 1 hour, cooling back test electrical property is as follows:
Surface load 6W/cm
2The time, leakage current is 0.010mA (switching on 20 minutes)
Surface load 8W/cm
2The time, leakage current is 0.0395mA (switching on 20 minutes)
The powder flow velocity: φ 4m/m aperture under meter, the time is 39.3s/100g
Compacted density: reach 2.21g/cm
3
More than relevant performance reached the performance requriements of high temperature electric heating tube to the insulation filling material.
Embodiment two:
(1). get tetraethyl silicate 100ml and put into container, under whipped state, add the 285ml dehydrated alcohol, and stirred 0.5 hour.
(2). other gets a 285ml dehydrated alcohol, is mixed into mixing solutions with 12g distilled water, 1.5g phosphoric acid.
(3). the mixing solutions in (2) step is slowly joined under whipped state in the container in (1) step, stirred simultaneously 1 hour.
(4). container is built, left standstill 24 hours, promptly form SiO
2Colloidal sol, stand-by.
(5). with above-mentioned SiO
2Colloidal sol stirs, and slowly adds the MgO powder after deironing and drying treatment simultaneously, stirs.Wherein, the add-on of MgO powder is 1800g.
(6). the material in (5) is dry under whipped state, treat that liquid disappears after, stop to stir.Then in baking oven 80 ℃ the oven dry 24 hours, make the material thorough drying.
(7). the material in (6) is put into alumina crucible, calcine in air atmosphere, calcining temperature is 700 ℃, is incubated 2 hours.
(8). cooled material in (7) is come out of the stove, and vibration mill 6 hours is the high temperature resisting electrothermal insulating magnesia material that the present invention prepares.
(9). the tubulature test:
MgO powder after the above-mentioned processing is packed in the electrothermal tube of test, and then 1000 ℃ of integrally annealeds 1 hour, cooling back test electrical property is as follows:
Surface load 6W/cm
2The time, leakage current is 0.010mA (switching on 20 minutes)
Surface load 8W/cm
2The time, leakage current is 0.038mA (switching on 20 minutes)
The powder flow velocity: φ 4m/m aperture under meter, the time is 39.5s/100g
Compacted density: reach 2.14g/cm
3
More than relevant performance reached the performance requriements of high temperature electric heating tube to the insulation filling material.
Embodiment three:
(1). get tetraethyl silicate 100ml and put into container, under whipped state, add the 200ml dehydrated alcohol, and stirred 0.5 hour.
(2). other gets a 200ml dehydrated alcohol, is mixed into mixing solutions with 15.5g distilled water, 2.0g phosphoric acid.
(3). the mixing solutions in (2) step is slowly joined under whipped state in the container in (1) step, stirred simultaneously 1 hour.
(4). container is built, left standstill 24 hours, promptly form SiO
2Colloidal sol, stand-by.
(5). with above-mentioned SiO
2Colloidal sol stirs, and slowly adds the MgO powder after deironing and drying treatment simultaneously, stirs.Wherein, the add-on of MgO powder is 1345g.
(6). the material in (5) is dry under whipped state, treat that liquid disappears after, stop to stir.Then in baking oven 80 ℃ the oven dry 24 hours, make the material thorough drying.
(7). the material in (6) is put into alumina crucible, calcine in air atmosphere, calcining temperature is 750 ℃, is incubated 2 hours.
(8). cooled material in (7) is come out of the stove, and vibration mill 6 hours is the high temperature resisting electrothermal insulating magnesia material that the present invention prepares.
(9). the tubulature test:
MgO powder after the above-mentioned processing is packed in the electrothermal tube of test, and then 1000 ℃ of integrally annealeds 1 hour, cooling back test electrical property is as follows:
Surface load 6W/cm
2The time, leakage current is 0.008mA (switching on 20 minutes)
Surface load 8W/cm
2The time, leakage current is 0.037mA (switching on 20 minutes)
The powder flow velocity: φ 4m/m aperture under meter, the time is 39.9s/100g
Compacted density: reach 2.10g/cm
3
More than relevant performance reached the performance requriements of high temperature electric heating tube to the insulation filling material.
Embodiment four:
(1). get tetraethyl silicate 100ml and put into container, under whipped state, add the 150ml dehydrated alcohol, and stirred 0.5 hour.
(2). other gets a 150ml dehydrated alcohol, is mixed into mixing solutions with 16g distilled water, 1.6g phosphoric acid.
(3). the mixing solutions in (2) step is slowly joined under whipped state in the container in (1) step, stirred simultaneously 1 hour.
(4). container is built, left standstill 24 hours, promptly form SiO
2Colloidal sol, stand-by.
(5). with above-mentioned SiO
2Colloidal sol stirs, and slowly adds the MgO powder after deironing and drying treatment simultaneously, stirs.Wherein, the add-on of MgO powder is 1100g.
(6). the material in (5) is dry under whipped state, treat that liquid disappears after, stop to stir.Then in baking oven 80 ℃ the oven dry 24 hours, make the material thorough drying.
(7). the material in (6) is put into alumina crucible, calcine in air atmosphere, calcining temperature is 800 ℃, is incubated 1.5 hours.
(8). cooled material in (7) is come out of the stove, and vibration mill 6 hours is the high temperature resisting electrothermal insulating magnesia material that the present invention prepares.
(9). the tubulature test:
MgO powder after the above-mentioned processing is packed in the electrothermal tube of test, and then 1000 ℃ of integrally annealeds 1 hour, cooling back test electrical property is as follows:
Surface load 6W/cm
2The time, leakage current is 0.0081mA (switching on 20 minutes)
Surface load 8W/cm
2The time, leakage current is 0.0376mA (switching on 20 minutes)
The powder flow velocity: φ 4m/m aperture under meter, the time is 39.5s/100g
Compacted density; Reach 2.15g/cm
3
More than relevant performance reached the performance requriements of high temperature electric heating tube to the insulation filling material.
Claims (1)
1, a kind of preparation method of high temperature resisting electrothermal insulating magnesia material is characterized in that, this method may further comprise the steps:
(1). dehydrated alcohol is joined in the container of placing tetraethyl silicate, stirred 0.5 hour, wherein, the alcoholic acid add-on is: tetraethyl silicate: (tetraethyl silicate+2 * ethanol)=0.1～0.3: 1, tetraethyl silicate and ethanol are volume unit;
(2). other gets dehydrated alcohol a and (1) step equal volume, is mixed into mixing solutions with distilled water, phosphoric acid, and wherein, the add-on of distilled water is in molar ratio: water: tetraethyl silicate=1～5: 1 calculates; The add-on of phosphoric acid is in molar ratio: phosphoric acid: tetraethyl silicate=0.01～0.1: 1 calculates;
(3). the mixing solutions in (2) step is slowly joined under whipped state in the container in (1) step, stirred simultaneously 1 hour, container is built, left standstill 24 hours, promptly form SiO
2Colloidal sol, stand-by;
(4). with above-mentioned SiO
2Colloidal sol stirs, slowly add simultaneously the MgO powder after deironing and drying treatment, stir, the add-on of MgO powder is: MgO=(5.38～53.8) * tetraethyl silicate * tetraethyl silicate proportion, wherein tetraethyl silicate is volume unit, and MgO is a mass unit;
(5). the material in (4) is dry under whipped state, treat that liquid disappears after, stop to stir, 80 ℃ of oven dry 24 hours in baking oven then make the material thorough drying;
(6). the material in (5) is put into alumina crucible, calcine in air atmosphere, calcining temperature is 600～1000 ℃, is incubated 1～6 hour, and after cooling was come out of the stove, vibration mill 6 hours was the high temperature resisting electrothermal insulating magnesia material that the present invention prepares.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 00130288 CN1117699C (en) | 2000-11-03 | 2000-11-03 | Preparation of high temperature resisting electrothermal insulating magnesia material |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 00130288 CN1117699C (en) | 2000-11-03 | 2000-11-03 | Preparation of high temperature resisting electrothermal insulating magnesia material |
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| CN1288859A CN1288859A (en) | 2001-03-28 |
| CN1117699C true CN1117699C (en) | 2003-08-13 |
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Families Citing this family (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP5447355B2 (en) * | 2010-12-02 | 2014-03-19 | 新神戸電機株式会社 | Method for producing thermosetting resin composition, method for producing prepreg and laminate |
| CN102786293B (en) * | 2012-07-26 | 2014-01-15 | 汪长安 | Production method for magnesium oxide insulating preform for mineral heating cables |
| CN105985533B (en) * | 2015-02-26 | 2018-10-02 | 宝山钢铁股份有限公司 | The method that orientation silicon steel magnesia waste manufactures supra polymer plastic additive |
| CN105037804A (en) * | 2015-06-30 | 2015-11-11 | 大连理工大学 | Preparation method of synergetic silicon-magnesium composite fire retardant with core-shell structure |
| CN106186007A (en) * | 2016-07-07 | 2016-12-07 | 安徽省含山县锦华氧化锌厂 | A kind of MgO granule with micron/nano composite construction and preparation method thereof |
| CN106187202A (en) * | 2016-07-14 | 2016-12-07 | 安徽樵森电气科技股份有限公司 | A kind of aluminium nitride ceramics insulator preparation method |
| CN109835927B (en) * | 2017-11-28 | 2021-09-17 | 中国科学院大连化学物理研究所 | High-temperature-resistant and high-hydrophobicity electric-grade magnesium oxide powder and preparation method thereof |
| CN111233012B (en) * | 2018-11-28 | 2021-10-08 | 中国科学院大连化学物理研究所 | Electrical-grade magnesium oxide powder and preparation method thereof |
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