CN102108567A - Method for preparing superfine magnesia ceramic fibers - Google Patents
Method for preparing superfine magnesia ceramic fibers Download PDFInfo
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- CN102108567A CN102108567A CN2009102487849A CN200910248784A CN102108567A CN 102108567 A CN102108567 A CN 102108567A CN 2009102487849 A CN2009102487849 A CN 2009102487849A CN 200910248784 A CN200910248784 A CN 200910248784A CN 102108567 A CN102108567 A CN 102108567A
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- gel
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- magnesia ceramic
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Abstract
The invention provides a method for preparing a superfine magnesia ceramic fiber. The method comprises the following steps: adopting citric acid and magnesium carbonate as raw materials to form a homogenous aqueous solution, conducting polycondensation on products subjected to hydrolyzation to prepare sol, dehydrating sol into gel, achieving a certain viscosity of gel, spinning at normal temperature to obtain gel white thread , drying white thread to obtain a precursor gel fiber, thermally treating the precursor gel fiber to remove water and organic matter, and making the superfine magnesia ceramic fiber with a smooth surface and a compact and netlike fiber structure under the condition of lower temperature. The superfine magnesia ceramic fiber has high purity and stable performance, and the diameter of the fiber can reach less than 1 micrometers. The method provided by the invention has the advantages of reasonable design, scientific configuration, simple process and convenience for operation.
Description
Technical field
The invention belongs to technical field of refractory materials, relate in particular to a kind of method of producing the super fine magnesia ceramic fibre.
Background technology
In recent years, the super fine magnesia ceramic fibre has obtained application more and more widely in fields such as refractory material, insulating materials and sound insulating materials simultaneously with the generally approval that corrosion-resistant, the heat-resisting ability and good heat-insulation and heat-preservation, sound insulation insulating properties and the thermal shock resistance of its excellence obtained industry.At present, the production method of super fine magnesia ceramic fibre mainly is to adopt direct oxidation sedimentation, slurry process etc., though these methods also can both be produced the magnesia ceramics fiber, but the common defective that exists of these methods is, employed equipment and Work tool are more, complex manufacturing, most importantly the diameter of the magnesia ceramics fiber produced of these methods is mostly more than micron order, can't prepare the following super fine magnesia ceramic fibre of submicron order, thereby the range of application of magnesia ceramics fiber and use field are limited to.
Summary of the invention
Purpose of the present invention is exactly at the problems referred to above, provides a kind of simple, is convenient to operation, can prepare the method for the super fine magnesia ceramic fibre of purity height, stable performance at a lower temperature.
For this reason, the solution that the present invention taked is:
A kind of preparation method of super fine magnesia ceramic fibre, with analytically pure citric acid and chemical pure magnesium carbonate is raw material, be dissolved in the deionized water than the ratio that is 2 and mix in the amount of substance of citric acid and magnesium ion, utilize magnetic stirrer 14-15h, and the pH value of control solution is between 4.5-5.0; Then the solution after the magnetic agitation is moved in the rotary evaporator, at 65-70 ℃ of following reduction vaporization dehydration, the colloidal sol that obtains having certain viscosity; Again the colloidal sol that makes is put into drying box, dry 7-8h under 70-80 ℃ of condition, but the gel of formation wire drawing; But utilize glass bar at the uniform velocity wire drawing from the gel of wire drawing, obtain the plain silk of gel; The plain silk of gel is placed baking oven,, obtain magnesia aqueous precursor gel fiber through 80-90 ℃ of dry 5h; At last the aqueous precursor gel fiber is placed crucible, make the super fine magnesia ceramic fibre behind the insulation 25min down at 470 ℃.
Beneficial effect of the present invention is:
The present invention is a raw material with citric acid and magnesium carbonate, adopt sol-gel process, and when gel reached certain viscosity, spinning at normal temperatures obtained plain of gel again, plain silk drying obtains the aqueous precursor gel fiber, the aqueous precursor gel fiber is removed moisture and organic matter, under lower temperature conditions again through Overheating Treatment, can make the super fine magnesia ceramic fibre of smooth surface, densification, reticular fiber structure, its purity height, stable performance, fibre diameter can reach below the 1 μ m.The inventive method is reasonable in design, the proportioning science, and technology is simple and be convenient to operation.
The specific embodiment
Below, the present invention will be further described in conjunction with the embodiments.
Embodiment 1:
Raw material is prepared: citric acid (analyzing pure) and magnesium carbonate (chemical pure);
Utensil is prepared: the lifting thermostat water bath, how to take into account electronic balance etc. with vavuum pump, rotary evaporator, air dry oven, magnetic stirring apparatus, pH value.
Be dissolved in the deionized water than the ratio that is 2 in the amount of substance of citric acid, and mix with magnesium ion.Utilize magnetic stirrer 14h, and the pH value of control solution is about 5.0.Then the solution after the magnetic agitation is moved in the rotary evaporator, at 65 ℃ of following reduction vaporization dehydrations, the colloidal sol that obtains having certain viscosity.The colloidal sol that makes is put into drying box, dry 7h under 80 ℃ of conditions, but the gel of formation wire drawing.Utilize glass bar from gel slowly, wire drawing evenly, obtain the plain silk of gel.The plain silk of gel is placed baking oven,, obtain magnesia aqueous precursor gel fiber through 80 ℃ of dry 5h; At last the aqueous precursor gel fiber is placed crucible, make the super fine magnesia ceramic fibre behind the insulation 25min down at 470 ℃.
Embodiment 2:
Raw material is prepared: citric acid (analyzing pure) and magnesium carbonate (chemical pure);
Utensil is prepared: the lifting thermostat water bath, how to take into account electronic balance etc. with vavuum pump, rotary evaporator, air dry oven, magnetic stirring apparatus, pH value.
Be dissolved in the deionized water than the ratio that is 2 and mix in the amount of substance of citric acid and magnesium ion, utilize magnetic stirrer 14.5h, and the pH value of control solution is about 4.5; Then the solution after the magnetic agitation is moved in the rotary evaporator, at 66 ℃ of following reduction vaporization dehydrations, the colloidal sol that obtains having certain viscosity; Again the colloidal sol that makes is put into drying box, dry 8h under 75 ℃ of conditions, but the gel of formation wire drawing; But utilize glass bar at the uniform velocity wire drawing from the gel of wire drawing, obtain the plain silk of gel; The plain silk of gel is placed baking oven,, obtain magnesia aqueous precursor gel fiber through 88 ℃ of dry 5h; At last the aqueous precursor gel fiber is placed crucible, make the super fine magnesia ceramic fibre behind the insulation 25min down at 470 ℃.
Claims (1)
1. the preparation method of a super fine magnesia ceramic fibre, it is characterized in that, with analytically pure citric acid and chemical pure magnesium carbonate is raw material, be dissolved in the deionized water than the ratio that is 2 and mix in the amount of substance of citric acid and magnesium ion, utilize magnetic stirrer 14-15h, and the pH value of control solution is between 4.5-5.0; Then the solution after the magnetic agitation is moved in the rotary evaporator, at 65-70 ℃ of following reduction vaporization dehydration, the colloidal sol that obtains having certain viscosity; Again the colloidal sol that makes is put into drying box, dry 7-8h under 70-80 ℃ of condition, but the gel of formation wire drawing; But utilize glass bar at the uniform velocity wire drawing from the gel of wire drawing, obtain the plain silk of gel; The plain silk of gel is placed baking oven,, obtain magnesia aqueous precursor gel fiber through 80-90 ℃ of dry 5h; At last the aqueous precursor gel fiber is placed crucible, make the super fine magnesia ceramic fibre behind the insulation 25min down at 470 ℃.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2009102487849A CN102108567A (en) | 2009-12-25 | 2009-12-25 | Method for preparing superfine magnesia ceramic fibers |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2009102487849A CN102108567A (en) | 2009-12-25 | 2009-12-25 | Method for preparing superfine magnesia ceramic fibers |
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| Publication Number | Publication Date |
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| CN102108567A true CN102108567A (en) | 2011-06-29 |
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| CN2009102487849A Pending CN102108567A (en) | 2009-12-25 | 2009-12-25 | Method for preparing superfine magnesia ceramic fibers |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102775148A (en) * | 2012-07-12 | 2012-11-14 | 东华大学 | Preparation method of magnesium diboride ceramic fiber precursor electrostatic spinning solution |
| CN103628181A (en) * | 2013-11-06 | 2014-03-12 | 华东师范大学 | Method for preparing magnesium oxide composite fiber |
| CN104404654A (en) * | 2014-12-15 | 2015-03-11 | 山东大学 | Method for preparing magnesium oxide fibers by ligand analysis technology |
| CN104446378A (en) * | 2014-12-15 | 2015-03-25 | 山东大学 | Spinning magnesium oxide fiber precursor sol as well as preparation method and application thereof |
| CN108892391A (en) * | 2018-09-17 | 2018-11-27 | 佛山皖和新能源科技有限公司 | A kind of preparation method of the anti-reflection membrane material of scratch resistant type |
| CN109111210A (en) * | 2018-09-17 | 2019-01-01 | 佛山皖和新能源科技有限公司 | A kind of preparation method of high-strength wearable type composite refractory |
| CN112431059A (en) * | 2020-10-29 | 2021-03-02 | 浙江鹏辰造纸研究所有限公司 | Temperature-resistant mineral fiber paper heat-insulating material and preparation method thereof |
-
2009
- 2009-12-25 CN CN2009102487849A patent/CN102108567A/en active Pending
Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102775148A (en) * | 2012-07-12 | 2012-11-14 | 东华大学 | Preparation method of magnesium diboride ceramic fiber precursor electrostatic spinning solution |
| CN103628181A (en) * | 2013-11-06 | 2014-03-12 | 华东师范大学 | Method for preparing magnesium oxide composite fiber |
| CN103628181B (en) * | 2013-11-06 | 2015-08-19 | 华东师范大学 | A kind of preparation method of magnesium oxide composite fiber |
| CN104404654A (en) * | 2014-12-15 | 2015-03-11 | 山东大学 | Method for preparing magnesium oxide fibers by ligand analysis technology |
| CN104446378A (en) * | 2014-12-15 | 2015-03-25 | 山东大学 | Spinning magnesium oxide fiber precursor sol as well as preparation method and application thereof |
| CN104404654B (en) * | 2014-12-15 | 2016-06-29 | 山东大学 | A kind of method adopting part analytic technique to prepare magnesia fibers |
| CN104446378B (en) * | 2014-12-15 | 2017-07-04 | 山东大学 | A kind of spinnability magnesia fibers precursor sol and preparation method and application |
| CN108892391A (en) * | 2018-09-17 | 2018-11-27 | 佛山皖和新能源科技有限公司 | A kind of preparation method of the anti-reflection membrane material of scratch resistant type |
| CN109111210A (en) * | 2018-09-17 | 2019-01-01 | 佛山皖和新能源科技有限公司 | A kind of preparation method of high-strength wearable type composite refractory |
| CN112431059A (en) * | 2020-10-29 | 2021-03-02 | 浙江鹏辰造纸研究所有限公司 | Temperature-resistant mineral fiber paper heat-insulating material and preparation method thereof |
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Application publication date: 20110629 |