CN102718495A - Magnesium silicon ceramic fiber and preparation method thereof - Google Patents
Magnesium silicon ceramic fiber and preparation method thereof Download PDFInfo
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- CN102718495A CN102718495A CN2012102087068A CN201210208706A CN102718495A CN 102718495 A CN102718495 A CN 102718495A CN 2012102087068 A CN2012102087068 A CN 2012102087068A CN 201210208706 A CN201210208706 A CN 201210208706A CN 102718495 A CN102718495 A CN 102718495A
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Abstract
The invention relates to a magnesium silicon ceramic fiber and a preparation method thereof. The invention adopts the technical scheme that the preparation method comprises the following steps of: mixing 1 to 10 weight percent of waste marble stone dust, 15 to 40 weight percent of forsterite powder, 2 to 8 weight percent of albite powder or potassium feldspar powder, 40 to 70 weight percent of quartz sand powder and 1 to 3 weight percent of industrial sodium tripolyphosphate which are used as the raw materials; pressing the mixture into a green body; carrying out heat treatment for 60 to 90minutes under the condition of a temperature of 1,000 to 1,300 DEG C; then crushing, grinding into 120 meshes, additionally adding the raw materials of 1 to 5 weight percent of industrial magnesium chloride and 0.5 to 3 weight percent of industrial starch and uniformly mixing the raw materials; then placing the uniformly mixed materials into a resistor furnace, heating to the temperature of 1,500 to 1,700 DEG C and throwing a thread after melting to obtain a ceramic fiber; and finally, carrying out heat treatment on the ceramic fiber for 1 to 4 hours under the condition of a temperature of 600 to 900 DEG C so as to obtain the magnesium silicon ceramic fiber. The magnesium silicon ceramic fiber and the preparation method thereof have the characteristics of low melting temperature, easiness for operating the fiber forming process and low production cost; and the prepared product has smooth surface, high mechanical strength, high using temperature and large biodegradation rate.
Description
Technical field
The invention belongs to the ceramic fiber technical field.Be specifically related to a kind of magnesium silicon ceramic fiber and preparation method thereof.
Background technology
The tradition alumina-silicate ceramic fibre produce, use and with the back unloading process in the fine dusts particle that produces, sucked respiratory system by human body after, very difficultly degraded by human body fluid, will bring out inflammation in respiratory system, even canceration.To losing the useless aluminum silicate fiber of use properties, adopt method processing such as landfill usually, because its stable chemical performance is difficult to be degraded, can pollute environment equally.Therefore, international cancer research association divides alumina-silicate ceramic fibre possibly classify by carcinogens into.The investigator has researched and developed the series product of dissolvable ceramics fiber in succession both at home and abroad, like magnesium silicon ceramic fiber.Normally raw material is through after the high-temperature fusion for magnesium silicon ceramic fiber, and the mode that adopts winding-up or get rid of silk prepares fiber; The magnesian existence of high level in fibrous makes it in human body fluid, have higher biodegradation rate; High level silicon-dioxide and magnesian existence made fiber have higher use temperature during such was fibrous.But the preparation and the performance of current magnesium silicon ceramic fiber still come with some shortcomings.Such as, limited by component characteristic, the melting raw materials TR is higher, viscosity of high-temperature melt is big, and becomes fine process medium viscosity rate of change wayward, thereby becomes the difficulty of fine operating process bigger; Fiber is prone to crystallization, efflorescence take place in the high temperature use, and then causes fiber reduction in work-ing life etc.
In addition, natural marble has produced a large amount of waste materials in the course of processing: stone material scrap stock and stone flour.At present, the stone material scrap stock have obtained utilizing fully again, but also do not have treatment process preferably for stone flour, can only it be piled up.The simple accumulation handled, and not only causes the waste of soil and resource, and can polluted source and local Air quality.Therefore, correct handling with utilize these stone powder waste materials, carry out the resource utilization reasonable development, have very important significance.
Become the big problem of fine operation easier in order to solve magnesium silicon ceramic fiber in producing at present; Usually in composition, introduce zirconium white, titanium oxide or rare-earth oxide; But what bring is the reduction of other performances of fiber thereupon, and, physical strength excessive or too small like Fibre diameter reduces, higher temperature line shrinks increase, biodegradation rate reduction etc.
In a word, in the technology of preparing of magnesium silicon ceramic fiber, still have certain deficiency at present: production cost is higher, the raw material temperature of fusion is higher, the fine process operation difficulty of one-tenth is big and the fiber use properties has much room for improvement etc.
Summary of the invention
The present invention is intended to overcome the deficiency of prior art, and purpose provides that a kind of production cost is low, temperature of fusion is lower and the preparation method of the magnesium silicon ceramic fiber that becomes fine process easy handling.The use temperature of the magnesium silicon ceramic fiber of this method preparation of usefulness is higher big with biodegradation rate.
For realizing above-mentioned purpose, the technical scheme that the present invention adopts is:
Be raw materials mix with the discarded marble stone flour of 1 ~ 10wt%, the forsterite powder of 15 ~ 40wt%, albite in powder or feldspar in powder, the quartz sand powder of 40 ~ 70wt% and the industrial tripoly phosphate sodium STPP of 1 ~ 3wt% of 2 ~ 8wt% earlier; Be pressed into base substrate, thermal treatment 60 ~ 90min under 1000 ~ 1300 ℃ of conditions;
Again that the material after the thermal treatment is broken, grinding to 120 order adds the industrial hex-ammoniate of said raw material 1 ~ 5wt% and the industrial starch of 0.5 ~ 3wt%, mixes;
Then the material that mixes is placed resistance furnace, be warming up to 1500 ~ 1700 ℃, directly get rid of silk after the fusion, obtain ceramic fiber;
With ceramic fiber thermal treatment 1 ~ 4 hour under 600 ~ 900 ℃ of conditions, promptly get magnesium silicon ceramic fiber at last.
In technique scheme:
The granularity of discarded marble stone flour is 80 ~ 120 orders, wherein CaCO
3Content is greater than 50wt%;
The granularity of forsterite powder is 40 ~ 120 orders; Its main chemical compositions is: SiO
2Be 25 ~ 35wt%, MgO is 50 ~ 65wt%, and CaO is 0.5 ~ 2wt%, Fe
2O
3Less than 8wt%;
The granularity of quartz sand powder is 40 ~ 120 orders; Its main chemical compositions is: SiO
2Be 90 ~ 99wt%, Fe
2O
3Less than 0.05wt%;
The granularity of albite in powder is 40 ~ 120 orders; Its main chemical compositions is: SiO
2Be 63 ~ 70wt%, Al
2O
3Be 16 ~ 25wt%, Na
2O is 9 ~ 15wt%;
The granularity of feldspar in powder is 40 ~ 120 orders; Its main chemical compositions is: SiO
2Be 64 ~ 69wt%, Al
2O
3Be 16 ~ 23wt%, K
2O is 9 ~ 18wt%;
The granularity of industry tripoly phosphate sodium STPP is 80 ~ 120 orders; Na wherein
5P
3O
10Content is greater than 90wt%;
The granularity of industrial hex-ammoniate is 80 ~ 120 orders; MgCl wherein
2Content is greater than 40wt%;
The pressure of compacting is 35 ~ 45MPa.
Because adopt technique scheme, the present invention compared with prior art has following positively effect:
1, temperature of fusion of the present invention is low, and it is mild to become the interior melt viscosity of fine scope to change, and becomes fine process to be easy to control;
2, the cost of material of the present invention's employing is cheap, and production cost is low, has very big industrialization prospect;
3, the long and slender dimension smooth surface of magnesium silicon pottery, the physical strength of the present invention's preparation are high, and use temperature is greater than 1200 ℃, and biodegradation rate is greater than 150ng/ (cm
2H).
Therefore, the present invention have temperature of fusion low, become fine process easy handling and the low characteristics of production cost; The smooth surface of prepared magnesium silicon ceramic fiber, physical strength are high, use temperature is higher and biodegradation rate is bigger.
Embodiment
Below in conjunction with embodiment the present invention being done further description, is not the restriction to its protection domain.
For avoiding repetition, the raw material unification with this embodiment earlier is described below, and repeats no more among each embodiment:
The granularity of discarded marble stone flour is 80 ~ 120 orders, wherein CaCO
3Content is greater than 50wt%;
The granularity of forsterite powder is 40 ~ 120 orders; Its main chemical compositions is: SiO
2Be 25 ~ 35wt%, MgO is 50 ~ 65wt%, and CaO is 0.5 ~ 2wt%, Fe
2O
3Less than 8wt%;
The granularity of quartz sand powder is 40 ~ 120 orders; Its main chemical compositions is: SiO
2Be 90 ~ 99wt%, Fe
2O
3Less than 0.05wt%;
The granularity of albite in powder is 40 ~ 120 orders; Its main chemical compositions is: SiO
2Be 63 ~ 70wt%, Al
2O
3Be 16 ~ 25wt%, Na
2O is 9 ~ 15wt%;
The granularity of feldspar in powder is 40 ~ 120 orders; Its main chemical compositions is: SiO
2Be 64 ~ 69wt%, Al
2O
3Be 16 ~ 23wt%, K
2O is 9 ~ 18wt%;
The granularity of industry tripoly phosphate sodium STPP is 80 ~ 120 orders; Na wherein
5P
3O
10Content is greater than 90wt%;
The granularity of industrial hex-ammoniate is 80 ~ 120 orders; MgCl wherein
2Content is greater than 40wt%;
The pressure of compacting is 35 ~ 45MPa.
Embodiment 1
A kind of magnesium silicon ceramic fiber and preparation method thereof.Be raw materials mix with the discarded marble stone flour of 6 ~ 10wt%, the forsterite powder of 30 ~ 40wt%, the quartz sand powder of 50 ~ 60wt%, the feldspar in powder of 2 ~ 5wt%, the industrial tripoly phosphate sodium STPP of 1 ~ 2wt% earlier; Be pressed into base substrate, thermal treatment 60 ~ 90min under 1000 ~ 1150 ℃ of conditions;
Again that the material after the thermal treatment is broken, grinding to 120 order adds the industrial hex-ammoniate of said raw material 1 ~ 3wt% and the industrial starch of 0.5 ~ 1.5wt%, mixes;
Then the material that mixes is placed resistance furnace, be warming up to 1500 ~ 1700 ℃, directly get rid of silk after the fusion, obtain ceramic fiber;
With ceramic fiber thermal treatment 2 ~ 3 hours under 800 ~ 900 ℃ of conditions, promptly get magnesium silicon ceramic fiber at last.
The magnesium silicon ceramic fiber that present embodiment is prepared: fiber surface is smooth, and physical strength is high, and use temperature is greater than 1200 ℃, and biodegradation rate is greater than 150ng/ (cm
2H).
Embodiment 2
A kind of magnesium silicon ceramic fiber and preparation method thereof.Be raw materials mix with the discarded marble stone flour of 1 ~ 4wt%, the forsterite powder of 15 ~ 25wt%, the quartz sand powder of 60 ~ 70wt%, the albite in powder of 4 ~ 8wt%, the industrial tripoly phosphate sodium STPP of 2 ~ 3wt% earlier; Be pressed into base substrate, thermal treatment 60 ~ 90min under 1100 ~ 1200 ℃ of conditions;
Again that the material after the thermal treatment is broken, grinding to 120 order adds the industrial hex-ammoniate of said raw material 2 ~ 4wt% and the industrial starch of 1 ~ 2wt%, mixes;
Then the material that mixes is placed resistance furnace, be warming up to 1500 ~ 1700 ℃, directly get rid of silk after the fusion, obtain ceramic fiber;
With ceramic fiber thermal treatment 3 ~ 4 hours under 600 ~ 700 ℃ of conditions, promptly get magnesium silicon ceramic fiber at last.
The magnesium silicon ceramic fiber that present embodiment is prepared: fiber surface is smooth, physical strength is high, and use temperature is greater than 1200 ℃, and biodegradation rate is greater than 180ng/ (cm
2H).
Embodiment 3
A kind of magnesium silicon ceramic fiber and preparation method thereof.Be raw materials mix with the discarded marble stone flour of 3 ~ 7wt%, the forsterite powder of 22 ~ 30wt%, the quartz sand powder of 56 ~ 65wt%, the albite in powder of 2 ~ 5wt%, the industrial tripoly phosphate sodium STPP of 1 ~ 2wt% earlier; Be pressed into base substrate, thermal treatment 60 ~ 90min under 1200 ~ 1300 ℃ of conditions;
Again that the material after the thermal treatment is broken, grinding to 120 order adds the industrial hex-ammoniate of said raw material 3 ~ 5wt% and the industrial starch of 2 ~ 3wt%, mixes;
Then the material that mixes is placed resistance furnace, be warming up to 1500 ~ 1700 ℃, directly get rid of silk after the fusion, obtain ceramic fiber;
With ceramic fiber thermal treatment 1 ~ 2 hour under 700 ~ 800 ℃ of conditions, promptly get magnesium silicon ceramic fiber at last.
The magnesium silicon ceramic fiber that present embodiment is prepared, fiber surface is smooth, physical strength is high, and use temperature is greater than 1200 ℃, and biodegradation rate is greater than 180ng/ (cm
2H).
Embodiment 4
A kind of magnesium silicon ceramic fiber and preparation method thereof.Be raw materials mix with the discarded marble stone flour of 8 ~ 10wt%, the forsterite powder of 35 ~ 40wt%, the quartz sand powder of 40 ~ 50wt%, the feldspar in powder of 4 ~ 8wt%, the industrial tripoly phosphate sodium STPP of 2 ~ 3wt% earlier; Be pressed into base substrate, thermal treatment 60 ~ 90min under 1000 ~ 1100 ℃ of conditions;
Again that the material after the thermal treatment is broken, grinding to 120 order adds the industrial hex-ammoniate of said raw material 1 ~ 2wt% and the industrial starch of 0.5 ~ 1wt%, mixes;
Then the material that mixes is placed resistance furnace, be warming up to 1500 ~ 1700 ℃, directly get rid of silk after the fusion, obtain ceramic fiber;
With ceramic fiber thermal treatment 2 ~ 3 hours under 600 ~ 700 ℃ of conditions, promptly get magnesium silicon ceramic fiber at last.
The magnesium silicon ceramic fiber that present embodiment is prepared, fiber surface is smooth, physical strength is high, and use temperature is greater than 1200 ℃, and biodegradation rate is greater than 200ng/ (cm
2H).
Embodiment 5
A kind of magnesium silicon ceramic fiber and preparation method thereof.Be raw materials mix with the discarded marble stone flour of 2 ~ 5wt%, the forsterite powder of 28 ~ 35wt%, the quartz sand powder of 55 ~ 65wt%, the feldspar in powder of 3 ~ 6wt%, the industrial tripoly phosphate sodium STPP of 1 ~ 2wt% earlier; Be pressed into base substrate, thermal treatment 60 ~ 90min under 1150 ~ 1250 ℃ of conditions;
Again that the material after the thermal treatment is broken, grinding to 120 order adds the industrial hex-ammoniate of said raw material 2 ~ 4wt% and the industrial starch of 2 ~ 3wt%, mixes;
Then the material that mixes is placed resistance furnace, be warming up to 1500 ~ 1700 ℃, directly get rid of silk after the fusion, obtain ceramic fiber;
With ceramic fiber thermal treatment 2 ~ 3 hours under 800 ~ 900 ℃ of conditions, promptly get magnesium silicon ceramic fiber at last.
The magnesium silicon ceramic fiber that present embodiment is prepared, fiber surface is smooth, physical strength is high, and use temperature is greater than 1200 ℃, and biodegradation rate is greater than 150ng/ (cm
2H).
Embodiment 6
A kind of magnesium silicon ceramic fiber and preparation method thereof.Be raw materials mix with the discarded marble stone flour of 7 ~ 9wt%, the forsterite powder of 30 ~ 40wt%, the quartz sand powder of 45 ~ 55wt%, the albite in powder of 3 ~ 7wt%, the industrial tripoly phosphate sodium STPP of 1 ~ 2wt% earlier; Be pressed into base substrate, thermal treatment 60 ~ 90min under 1200 ~ 1300 ℃ of conditions;
Again that the material after the thermal treatment is broken, grinding to 120 order adds the industrial hex-ammoniate of said raw material 4 ~ 5wt% and the industrial starch of 1 ~ 2wt%, mixes;
Then the material that mixes is placed resistance furnace, be warming up to 1500 ~ 1700 ℃, directly get rid of silk after the fusion, obtain ceramic fiber;
With ceramic fiber thermal treatment 3 ~ 4 hours under 700 ~ 800 ℃ of conditions, promptly get magnesium silicon ceramic fiber at last.
The magnesium silicon ceramic fiber that present embodiment is prepared, fiber surface is smooth, physical strength is high, and use temperature is greater than 1200 ℃, and biodegradation rate is greater than 200ng/ (cm
2H).
This embodiment compared with prior art has following positively effect:
1, the temperature of fusion of this embodiment is low, and it is mild to become the interior melt viscosity of fine scope to change, and becomes fine process to be easy to control;
2, the cost of material of this embodiment employing is cheap, and production cost is low, has very big industrialization prospect;
3, the long and slender dimension smooth surface of magnesium silicon pottery, the physical strength of the preparation of this embodiment are high, and use temperature is greater than 1200 ℃, and biodegradation rate is greater than 150ng/ (cm
2H).
Therefore, this embodiment have temperature of fusion low, become fine process easy handling and the low characteristics of production cost; The smooth surface of prepared magnesium silicon ceramic fiber, physical strength are high, use temperature is higher and biodegradation rate is bigger.
Claims (10)
1. the preparation method of a magnesium silicon ceramic fiber; It is characterized in that being raw materials mix with the discarded marble stone flour of 1 ~ 10wt%, the forsterite powder of 15 ~ 40wt%, albite in powder or feldspar in powder, the quartz sand powder of 40 ~ 70wt% and the industrial tripoly phosphate sodium STPP of 1 ~ 3wt% of 2 ~ 8wt% earlier; Be pressed into base substrate, thermal treatment 60 ~ 90min under 1000 ~ 1300 ℃ of conditions;
Again that the material after the thermal treatment is broken, grinding to 120 order adds the industrial hex-ammoniate of said raw material 1 ~ 5wt% and the industrial starch of 0.5 ~ 3wt%, mixes;
Then the material that mixes is placed resistance furnace, be warming up to 1500 ~ 1700 ℃, directly get rid of silk after the fusion, obtain ceramic fiber;
With ceramic fiber thermal treatment 1 ~ 4 hour under 600 ~ 900 ℃ of conditions, promptly get magnesium silicon ceramic fiber at last.
2. the preparation method of magnesium silicon ceramic fiber according to claim 1, the granularity that it is characterized in that said discarded marble stone flour is 80 ~ 120 orders, wherein CaCO
3Content is greater than 50wt%.
3. the preparation method of magnesium silicon ceramic fiber according to claim 1, the granularity that it is characterized in that said forsterite powder is 40 ~ 120 orders; Its main chemical compositions is: SiO
2Be 25 ~ 35wt%, MgO is 50 ~ 65wt%, and CaO is 0.5 ~ 2wt%, Fe
2O
3Less than 8wt%.
4. the preparation method of magnesium silicon ceramic fiber according to claim 1, the granularity that it is characterized in that said quartz sand powder is 40 ~ 120 orders; Its main chemical compositions is: SiO
2Be 90 ~ 99wt%, Fe
2O
3Less than 0.05wt%.
5. the preparation method of magnesium silicon ceramic fiber according to claim 1, the granularity that it is characterized in that said albite in powder is 40 ~ 120 orders; Its main chemical compositions is: SiO
2Be 63 ~ 70wt%, Al
2O
3Be 16 ~ 25wt%, Na
2O is 9 ~ 15wt%.
6. the preparation method of magnesium silicon ceramic fiber according to claim 1, the granularity that it is characterized in that said feldspar in powder is 40 ~ 120 orders; Its main chemical compositions is: SiO
2Be 64 ~ 69wt%, Al
2O
3Be 16 ~ 23wt%, K
2O is 9 ~ 18wt%.
7. the preparation method of magnesium silicon ceramic fiber according to claim 1, the granularity that it is characterized in that said industrial tripoly phosphate sodium STPP is 80 ~ 120 orders; Na wherein
5P
3O
10Content is greater than 90wt%.
8. the preparation method of magnesium silicon ceramic fiber according to claim 1, the pressure that it is characterized in that said compacting is 35 ~ 45MPa.
9. the preparation method of magnesium silicon ceramic fiber according to claim 1, the granularity that it is characterized in that said industrial hex-ammoniate is 80 ~ 120 orders; MgCl wherein
2Content is greater than 40wt%.
10. according to the prepared magnesium silicon ceramic fiber of preparation method of each described magnesium silicon ceramic fiber in the claim 1 ~ 9.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103820881A (en) * | 2014-02-08 | 2014-05-28 | 北京大学 | Method for preparing ceramic fibers from high-aluminum fly ash |
| CN105198226A (en) * | 2015-09-10 | 2015-12-30 | 武汉科技大学 | Forsterite fiber and preparation method thereof |
| CN104649692B (en) * | 2015-01-16 | 2016-08-17 | 长兴正发热电耐火材料有限公司 | A kind of high chromium ceramic fibre and preparation method thereof |
| CN106350901A (en) * | 2016-08-26 | 2017-01-25 | 宜兴润德纺织品制造有限公司 | Compound waterproof fiber for weaving textile fabric and preparation method thereof |
| CN108677272A (en) * | 2018-05-15 | 2018-10-19 | 华南理工大学 | A kind of micro inorganic anti-bacterial fibre and preparation method thereof |
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| CN102491737A (en) * | 2011-12-08 | 2012-06-13 | 武汉科技大学 | High-temperature-resistant biologically-soluble ceramic fiber and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102491737A (en) * | 2011-12-08 | 2012-06-13 | 武汉科技大学 | High-temperature-resistant biologically-soluble ceramic fiber and preparation method thereof |
Non-Patent Citations (1)
| Title |
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| 姜广坤等: "氯化物对钙镁硅可溶耐火纤维析晶和溶解行为的影响", 《武汉科技大学学报》 * |
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103820881A (en) * | 2014-02-08 | 2014-05-28 | 北京大学 | Method for preparing ceramic fibers from high-aluminum fly ash |
| CN103820881B (en) * | 2014-02-08 | 2015-12-02 | 北京大学 | A kind of method utilizing aluminous fly-ash to prepare ceramic fibre |
| CN104649692B (en) * | 2015-01-16 | 2016-08-17 | 长兴正发热电耐火材料有限公司 | A kind of high chromium ceramic fibre and preparation method thereof |
| CN105198226A (en) * | 2015-09-10 | 2015-12-30 | 武汉科技大学 | Forsterite fiber and preparation method thereof |
| CN106350901A (en) * | 2016-08-26 | 2017-01-25 | 宜兴润德纺织品制造有限公司 | Compound waterproof fiber for weaving textile fabric and preparation method thereof |
| CN108677272A (en) * | 2018-05-15 | 2018-10-19 | 华南理工大学 | A kind of micro inorganic anti-bacterial fibre and preparation method thereof |
| CN108677272B (en) * | 2018-05-15 | 2020-09-22 | 华南理工大学 | Micron-sized inorganic antibacterial fiber and preparation method thereof |
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| CN102718495B (en) | 2013-12-04 |
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