CN109835927A - A kind of high temperature resistant, Gao Shushui fused magnesium oxide powder and preparation method thereof - Google Patents
A kind of high temperature resistant, Gao Shushui fused magnesium oxide powder and preparation method thereof Download PDFInfo
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Abstract
The present invention provides a kind of high temperature resistant, Gao Shushui fused magnesium oxide powder and preparation method thereof.The feature of product of the present invention is, is high-purity magnesium oxide inside particle, and outside is inorganic oxide silicon coating.Its preparation process includes: the fused magnesite for crushing and screening certain mesh number, it is grown with there is the ageing of silicon solution.This method concrete operations are as follows: crushing and screening fused magnesite；At least one organic silicon solvent is added again and fused magnesite is mixed；Then inducer is added；Filtering, drying after ageing a period of time, finally high temperature resistant, Gao Shushui fused magnesium oxide powder can be obtained in roasting.Operation of the present invention is simple, consumes energy low, the fused magnesium oxide of preparation has superior hydrophobicity and heat-resisting quantity.
Description
Technical field
The present invention relates to field of material preparation, and in particular to a kind of high temperature resistant, Gao Shushui fused magnesium oxide powder and its system
Preparation Method.
Background technique
Fused magnesium oxide powder has excellent insulating properties and heat-conductive characteristic, and being mainly used for production has heating function
Electric elements.Electrically molten magnesia sand then passes through a series of electrician's grade oxygen of process for producing by crushing, processing and grain size proportion
Change magnesium powder
It can be widely used in the insulation filling material of heating element.
The factor for influencing fused magnesium oxide powder mainly has thermal conductivity, dielectric strength, hydroscopicity, aquation rate, magnetization object to contain
Amount etc..Since the raw material of fused magnesium oxide powder is mainly derived from fused magnesite, fused magnesite content of magnesia in the market is low,
Hydroscopicity is big, aquation rate is high, and the electric property of heating element can be damaged after use, is easy electric leakage even booster, there are great peaces
Full hidden danger.In addition, prepared by heating element may contain a small amount of organic matter in material and filler, organic matter can divide under high temperature
Solution, is carbonized and leads to magnesia blackening at diffusion, to influence heating element electric property.The hydrophobic fused magnesium oxide of high temperature resistant
Powder using very extensive, it is civilian to be primarily adapted for use in: the top grade stainless steel tube, English such as microwave boiler tube, bread producing machine pipe, oven heat pipe
On Ge Lai pipe, the insulation performance under high temperature is directly related to the superiority and inferiority of electric heating products.High-end product can also be used in make aviation,
The fields such as space flight, nuclear power insulating materials.
Currently, Chinese patent CN107204213A discloses a kind of production method of fused magnesium oxide powder, specific steps
It is as follows: fused magnesite to be crushed, screening process, base extraction；The inorganic fillers such as kaolin are added after drying again, are sieved
Except magnetic；Fused magnesium oxide powder is arrived to magnesia powder surface sprinkling silicone oil finally by spray pattern.Patent
CN16967309A discloses a kind of production method of pot water aluminum pipe electrician's grade magnesia powder, first by electric smelting MAG block grinding screen
Point, addition organosilicon material mixing, normal temperature cure, then add inorganic nano material and do oil absorbent, it is solid in 80~150 degree of kilns
Change, natural cooling is to get to fused magnesium oxide powder after last 200~250 degree hot settings.Patent CN103922615A is disclosed
A kind of method that rudimentary electrically molten magnesia is prepared into advanced fused magnesium oxide.Capacitive oxidation magnesium powder is heated to 800~
2000 degree, quenching is carried out after held for some time, and fused magnesium oxide powder can be obtained.Patent CN103523791B is disclosed
A kind of preparation method of fused magnesium oxide additive, can be greatly reduced electrician after mixing using this additive with electrically molten magnesia
The leakage current of grade high-temperature oxydation magnesium.Detailed process is as follows: first mixing a certain proportion of magnesia with silica and high
Temperature calcining, it is then cooling, then boron compound mixing is added, passing through high-temperature calcination.Last obtained cooled material crushes and screens
Obtain required product.It is a kind of disclosed in patent CN103971786B to prepare electric oven electrician's grade organic coating high-temperature insulation
The method of magnesia powder, the heating element of the production need not move through 1050 degree of annealing.Patent US4677026 discloses one
The preparation method of the moisture-proof fused magnesium oxide powder of kind is passed through 600 degree of organosilicons in the fluidized bed containing electrically molten magnesia and steams
Vapour is covered on electrically molten magnesia particle surface after organosilicon pyrolysis, to form damp proof insulation fused magnesium oxide powder product.
China has evolved into the manufacture base of global household electrical appliances, at the same heavy chemical industry, aerospace production field also by
Flaring is big, while China is also the production base of electric insulating material.But since current technology falls behind, equipment is unqualified, leads
The fused magnesium oxide for causing China to produce is not only at high cost, product quality is low, and generally based on middle low-temperature oxidation magnesium powder.Therefore
The fused magnesium oxide powder that it is good that development & production goes out high-quality high temperature resistant, moisture resistance has become a top priority.
Summary of the invention
For the heat-resisting quantity for being difficult to overcome fused magnesium oxide powder of patent disclosed above, and high temperature resistant electrical grade aoxidizes
The preparation process of magnesium is complicated, and it is big to consume energy, and environmental pollution is serious.In order to overcome the disadvantage and deficiency in the above-mentioned prior art,
The present invention provides a kind of high temperature resistant, Gao Shushui fused magnesium oxide powder and preparation method thereof.
The fused magnesium oxide powder of a kind of high temperature resistant of the present invention, high hydrophobicity, internal is high-purity magnesium oxide, and outside is nothing
Machine silica dioxide coating.
A kind of high temperature resistant of the present invention, Gao Shushui fused magnesium oxide powder, the inside of the fused magnesium oxide powder are high-purity
Magnesia, the purity of magnesia are 96-99.9%；
A kind of high temperature resistant of the present invention, Gao Shushui fused magnesium oxide powder, the outside inorganic two of the fused magnesium oxide powder
Silica coating with a thickness of 0.1~100nm；Siliconoxide mass and magnesia mass ratio are between 0.1~10%；
A kind of high temperature resistant, high hydrophobicity fused magnesium oxide powder preparation method, realized by following step:
(1) fused magnesite is crushed to 40 mesh~325 mesh, electrically molten magnesia powder, content of magnesia 95~98% is made；
(2) organic silicon solution and alcohols solvent are mixed, and are sufficiently stirred, be configured to solution A；
(3) alkaline inducer, deionized water and alcohols solvent are mixed again, and are sufficiently stirred, be configured to solution B；
(4) electrically molten magnesia powder made of step (1) and solution A are mixed and stirred for 20~30 minutes, slurry C is made；
(5) solution B is added into slurry C within a certain period of time, with certain proportion, is stirred evenly；
(6) it under the conditions of 20~80 degree, is aged 30~180 minutes, stands filtering；
(7) filtered solid particle is 5~24 hours dry under the conditions of 40~200 degree；
(8) solid roasts 2~10 hours under the conditions of 800~2000 degree after will be dry.
Organic silicon solution described in step (2) is selected from methyl orthosilicate, ethyl orthosilicate, positive silicic acid propyl ester, positive silicic acid fourth
One or more of ester.
Step (2) alcohols is selected from methanol, ethyl alcohol, normal propyl alcohol, isopropanol, one or more of ethylene glycol.
Step (3) the alkaline inducer is selected from sodium hydroxide, potassium hydroxide, sodium carbonate, ammonium hydroxide, triethylamine, in pyridine
One or more.
Step (3) alcohols is selected from methanol, ethyl alcohol, normal propyl alcohol, isopropanol, one or more of ethylene glycol.
Feed time range described in step (5) is 1~120 minute.
Step (5) described mixed proportion: the molar ratio of organic silicon solution (in terms of SiO2), alkaline inducer and deionized water
For 1:(0.001~100): (1~600).
The present invention for the prior art have the following advantages and the utility model has the advantages that
1. high temperature resistant prepared by the present invention, Gao Shushui fused magnesium oxide can tolerate 2000 degree of high temperature, and damp proof insulation performance >
1000MΩ。
2. operation of the present invention is simple, consume energy low, not generation environment pollutant.
3. easily amplification industrialization of the invention, without cumbersome last handling process, substantially lowers production cost.
Detailed description of the invention
Fig. 1 is preparation flow figure of the invention.
Specific embodiment
Specific embodiments of the present invention are further described in detail for son with reference to the accompanying drawings and examples, but these
Embodiment does not limit the invention.Those skilled in the art can be to technical solution of the present invention in spirit of the present invention
Details and form modify, but these modifications are fallen within the protection scope of the present invention.
For more convenient understanding and show that the present invention, preparation flow figure of the invention are as shown in Figure 1.The high temperature resistant of this sample
It with waterproofing tests is completed in the SU304 stainless steel tube that diameter is 6.6mm, length is 500mm, the heating of electric furnace silk
Power is 500W.Hydrophobicity test is to test its insulation performance in the case where humidity is respectively 50% 90%.
Embodiment 1
Fused magnesite is crushed to and is sized to 40 mesh~325 mesh, electrically molten magnesia powder is made.Electrically molten magnesia powder 1kg is taken,
Ethyl orthosilicate 50g, ethyl alcohol 2kg, stirs and slurry is made；Concentrated ammonia liquor 3g is taken, ethyl alcohol 3kg is sufficiently mixed, and is added
Into magnesia powder slurry, the time was controlled at 30 minutes.It after charging, is aged 1 hour in 50 degree of water-baths, stands filtering.
The solid that will filter out is put into baking oven, and 150 degree of conditions are 10 hours dry.To natural cooling, place under the conditions of 1200 degree of kiln
Roasting 6 hours.Products obtained therefrom is tested by SEM, and for silica coating with a thickness of 35nm, SiO2 content is the 2.1% of MgO.
Embodiment 2
Fused magnesite is crushed to and is sized to 40 mesh~325 mesh, electrically molten magnesia powder is made.Take electrically molten magnesia powder
0.5kg, methyl orthosilicate 150g, methanol 3kg are stirred and slurry are made；Concentrated ammonia liquor 1.5g is taken, methanol 5kg is sufficiently mixed
It closes, and is added into magnesia powder slurry, the time controlled at 55 minutes.After charging, it is aged 3 hours in 30 degree of water-baths,
Stand filtering.The solid that will filter out is put into baking oven, and 40 degree of conditions are 24 hours dry.To natural cooling, kiln 1100 is placed into
It is roasted 10 hours under the conditions of degree.Products obtained therefrom is tested by SEM, and for silica coating with a thickness of 40nm, SiO2 content is MgO's
1.6%.
Embodiment 3
Fused magnesite is crushed to and is sized to 40 mesh~325 mesh, electrically molten magnesia powder is made.Take electrically molten magnesia powder
3.2kg, ethyl orthosilicate 80g, ethyl alcohol 4.5kg are stirred and slurry are made；Concentrated ammonia liquor 6.5g, ethyl alcohol 2.6kg is taken to fill
Divide mixing, and be added into magnesia powder slurry, the time controlled at 35 minutes.After charging, it is small that 2 are aged in 80 degree of water-baths
When, stand filtering.The solid that will filter out is put into baking oven, and 60 degree of conditions are 24 hours dry.To natural cooling, kiln is placed into
It is roasted 3 hours under the conditions of 1800 degree.Products obtained therefrom is tested by SEM, and silica coating is with a thickness of 30nm, SiO2 content
The 1.1% of MgO.
High temperature resistant made of the embodiment of the present invention 1,2,3, Gao Shushui fused magnesium oxide powder and general uncoated electrician's grade
Magnesia powder is made comparisons, and after being fabricated to standard heating element respectively, tests its component content, mesh number analysis and electric insulating quality
Analysis, comparing result is as shown in table 1, table 2, table 3.
Each embodiment constituent analysis table of table 1
| Sample lot number | MgO | CaO | Fe2O3 | SiO2 | Al2O3 | L.O.I |
| Embodiment 1 | 95.93 | 0.67 | 0.36 | 2.75 | 0.26 | 0.03 |
| Embodiment 2 | 95.84 | 0.67 | 0.36 | 2.85 | 0.26 | 0.02 |
| Embodiment 3 | 96.34 | 0.56 | 0.36 | 2.45 | 0.26 | 0.03 |
| Uncoated MgO | 97.02 | 0.82 | 0.4 | 1.46 | 0.26 | 0.04 |
Each embodiment mesh number analytical table (content %) of table 2
Each embodiment electrical insulation properties analytical table (M Ω) of table 3
| Sample insulation performance | Normality | Damp state |
| Embodiment 1 | 3500 | 3500 |
| Embodiment 2 | 4500 | 4000 |
| Embodiment 3 | 4000 | 3500 |
| Uncoated MgO | 40 | 15 |
Note: sample pipe SU304 steel pipeLength: 500mm 110V/500W.
Claims (10)
1. the fused magnesium oxide powder of a kind of high temperature resistant, high hydrophobicity, it is characterised in that: be height inside the fused magnesium oxide powder
Pure zirconia magnesium, outside are inorganic silicon dioxide coating.
2. according to claim 1 a kind of high temperature resistant, high hydrophobicity fused magnesium oxide powder, it is characterised in that: electricity Gong Ji
The inside of magnesia powder is high-purity magnesium oxide, and the purity of magnesia is 96-99.9%.
3. according to claim 1 a kind of high temperature resistant, high hydrophobicity fused magnesium oxide powder, it is characterised in that: electricity Gong Ji
The external inorganic silicon dioxide coating of magnesia powder with a thickness of 0.1~100nm；Siliconoxide mass is with magnesia mass ratio
0.1~10%.
4. a kind of high temperature resistant, the preparation method of Gao Shushui fused magnesium oxide powder according to claim 1, it is characterised in that:
It follows the steps below:
(1) fused magnesite is crushed to 40 mesh~325 mesh, electrically molten magnesia powder, content of magnesia 95~98% is made；
(2) organic silicon solution and alcohols solvent are mixed, and are sufficiently stirred, be configured to solution A；
(3) alkaline inducer, deionized water and alcohols solvent are mixed again, and are sufficiently stirred, be configured to solution B；
(4) electrically molten magnesia powder made of step (1) and solution A are mixed and stirred for 20~30 minutes, slurry C is made；
(5) solution B is added into slurry C within a certain period of time, with certain proportion, is stirred evenly；
(6) it under the conditions of 20~80 degree, is aged 30~180 minutes, stands filtering；
(7) filtered solid particle is 5~24 hours dry under the conditions of 40~200 degree；
(8) solid roasts 2~10 hours under the conditions of 800~2000 degree after will be dry.
5. the preparation method of high temperature resistant according to claim 4, Gao Shushui fused magnesium oxide powder, it is characterised in that: step
Suddenly organic silicon solution described in (2) is selected from methyl orthosilicate, ethyl orthosilicate, one of positive silicic acid propyl ester or butyl silicate
Or it is several.
6. the preparation method of high temperature resistant according to claim 4, Gao Shushui fused magnesium oxide powder, it is characterised in that: step
Suddenly (2) described alcohols is selected from methanol, ethyl alcohol, normal propyl alcohol, isopropanol, one or more of ethylene glycol.
7. the preparation method of high temperature resistant according to claim 4, Gao Shushui fused magnesium oxide powder, it is characterised in that: step
Suddenly (3) described alkaline inducer is selected from sodium hydroxide, potassium hydroxide, sodium carbonate, ammonium hydroxide, one of triethylamine or pyridine or several
Kind.
8. the preparation method of high temperature resistant according to claim 4, Gao Shushui fused magnesium oxide powder, it is characterised in that: step
Suddenly (3) described alcohols is selected from methanol, ethyl alcohol, normal propyl alcohol, one or more of isopropanol or ethylene glycol.
9. the preparation method of high temperature resistant according to claim 4, Gao Shushui fused magnesium oxide powder, it is characterised in that: step
Suddenly feed time range described in (5) is 1~120 minute.
10. the preparation method of high temperature resistant according to claim 4, Gao Shushui fused magnesium oxide powder, it is characterised in that: step
Suddenly (5) mixed proportion: organic silicon solution is with SiO2The molar ratio of meter, alkaline inducer and deionized water be 1:0.001~
100:1~600, volume ratio of the alcohols solvent in total solution are 60~85%.
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN110255589A (en) * | 2019-07-17 | 2019-09-20 | 辽宁嘉顺化工科技有限公司 | A kind of preparation method and process units of moisture-proof hydrophobicity medium temperature fused magnesium oxide powder |
| CN111718184A (en) * | 2020-05-18 | 2020-09-29 | 大石桥市美尔镁制品有限公司 | Magnesium oxide powder for calcining high-temperature oven, preparation method and application thereof |
| CN113582669A (en) * | 2021-07-30 | 2021-11-02 | 大石桥市美尔镁制品有限公司 | Magnesium oxide powder for calcining water heater, preparation method and application thereof |
| CN113652100A (en) * | 2021-08-16 | 2021-11-16 | 辽宁嘉顺科技有限公司 | Coated electrical magnesia with dioxane as coating diluent, and preparation method and application thereof |
| CN114106587A (en) * | 2021-12-13 | 2022-03-01 | 辽宁科技大学 | Method for preparing electrical-grade coated magnesium oxide by using environment-friendly ester solvent |
| CN114188109A (en) * | 2021-12-07 | 2022-03-15 | 辽宁嘉顺科技有限公司 | Preparation method and application of magnesium oxide for high-impedance and high-voltage breakdown prevention mineral insulated cable |
| CN117945738A (en) * | 2024-03-26 | 2024-04-30 | 辽宁嘉顺科技有限公司 | Preparation method of heat-conducting insulating magnesium oxide for high-temperature-resistant heating tube |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN114188109A (en) * | 2021-12-07 | 2022-03-15 | 辽宁嘉顺科技有限公司 | Preparation method and application of magnesium oxide for high-impedance and high-voltage breakdown prevention mineral insulated cable |
| CN114188109B (en) * | 2021-12-07 | 2024-05-10 | 辽宁嘉顺科技有限公司 | Preparation method and application of magnesium oxide for high-impedance high-voltage breakdown prevention mineral insulated cable |
| CN114106587A (en) * | 2021-12-13 | 2022-03-01 | 辽宁科技大学 | Method for preparing electrical-grade coated magnesium oxide by using environment-friendly ester solvent |
| CN117945738A (en) * | 2024-03-26 | 2024-04-30 | 辽宁嘉顺科技有限公司 | Preparation method of heat-conducting insulating magnesium oxide for high-temperature-resistant heating tube |
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