CN117888235A - Soluble ceramic fiber and preparation method thereof - Google Patents
Soluble ceramic fiber and preparation method thereof Download PDFInfo
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- CN117888235A CN117888235A CN202410078765.0A CN202410078765A CN117888235A CN 117888235 A CN117888235 A CN 117888235A CN 202410078765 A CN202410078765 A CN 202410078765A CN 117888235 A CN117888235 A CN 117888235A
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- fiber
- soluble ceramic
- ceramic fiber
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- 239000000835 fiber Substances 0.000 title claims abstract description 104
- 239000000919 ceramic Substances 0.000 title claims abstract description 37
- 238000002360 preparation method Methods 0.000 title abstract description 7
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 23
- 239000003245 coal Substances 0.000 claims abstract description 15
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims abstract description 11
- 239000000377 silicon dioxide Substances 0.000 claims abstract description 10
- KKCBUQHMOMHUOY-UHFFFAOYSA-N Na2O Inorganic materials [O-2].[Na+].[Na+] KKCBUQHMOMHUOY-UHFFFAOYSA-N 0.000 claims abstract description 6
- 229910052681 coesite Inorganic materials 0.000 claims abstract description 6
- 229910052593 corundum Inorganic materials 0.000 claims abstract description 6
- 229910052906 cristobalite Inorganic materials 0.000 claims abstract description 6
- 229910052682 stishovite Inorganic materials 0.000 claims abstract description 6
- 229910052905 tridymite Inorganic materials 0.000 claims abstract description 6
- 229910001845 yogo sapphire Inorganic materials 0.000 claims abstract description 6
- CPLXHLVBOLITMK-UHFFFAOYSA-N Magnesium oxide Chemical compound [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 claims description 36
- 239000000395 magnesium oxide Substances 0.000 claims description 18
- 238000000034 method Methods 0.000 claims description 16
- 239000010459 dolomite Substances 0.000 claims description 12
- 229910000514 dolomite Inorganic materials 0.000 claims description 12
- 238000002844 melting Methods 0.000 claims description 10
- 230000008018 melting Effects 0.000 claims description 10
- 229920000742 Cotton Polymers 0.000 claims description 8
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 claims description 7
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 claims description 7
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 7
- 239000011575 calcium Substances 0.000 claims description 7
- 229910052791 calcium Inorganic materials 0.000 claims description 7
- 239000011777 magnesium Substances 0.000 claims description 7
- 229910052749 magnesium Inorganic materials 0.000 claims description 7
- 229910052710 silicon Inorganic materials 0.000 claims description 7
- 239000010703 silicon Substances 0.000 claims description 7
- 238000009987 spinning Methods 0.000 claims description 7
- 239000002245 particle Substances 0.000 claims description 5
- 229910004298 SiO 2 Inorganic materials 0.000 claims description 4
- 239000010456 wollastonite Substances 0.000 claims description 4
- 229910052882 wollastonite Inorganic materials 0.000 claims description 4
- 235000008733 Citrus aurantifolia Nutrition 0.000 claims description 3
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 claims description 3
- 239000006004 Quartz sand Substances 0.000 claims description 3
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 claims description 3
- 235000011941 Tilia x europaea Nutrition 0.000 claims description 3
- 229910052839 forsterite Inorganic materials 0.000 claims description 3
- 239000004571 lime Substances 0.000 claims description 3
- HCWCAKKEBCNQJP-UHFFFAOYSA-N magnesium orthosilicate Chemical compound [Mg+2].[Mg+2].[O-][Si]([O-])([O-])[O-] HCWCAKKEBCNQJP-UHFFFAOYSA-N 0.000 claims description 3
- 238000002156 mixing Methods 0.000 claims description 3
- 239000011574 phosphorus Substances 0.000 claims description 3
- 229910052698 phosphorus Inorganic materials 0.000 claims description 3
- 239000011593 sulfur Substances 0.000 claims description 3
- 229910052717 sulfur Inorganic materials 0.000 claims description 3
- 239000000126 substance Substances 0.000 abstract description 6
- 241000219146 Gossypium Species 0.000 description 7
- 230000000052 comparative effect Effects 0.000 description 4
- 239000002657 fibrous material Substances 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- 239000000428 dust Substances 0.000 description 2
- 230000001105 regulatory effect Effects 0.000 description 2
- 229920002748 Basalt fiber Polymers 0.000 description 1
- 230000006978 adaptation Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 210000001124 body fluid Anatomy 0.000 description 1
- 239000010839 body fluid Substances 0.000 description 1
- 239000002817 coal dust Substances 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 239000012530 fluid Substances 0.000 description 1
- 239000003365 glass fiber Substances 0.000 description 1
- 239000012784 inorganic fiber Substances 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 230000007935 neutral effect Effects 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 235000012239 silicon dioxide Nutrition 0.000 description 1
- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical compound [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 description 1
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- Inorganic Fibers (AREA)
Abstract
The invention provides a soluble ceramic fiber, which comprises the following components ：SiO2：62～68wt％;Al2O3：＜3wt％;CaO：25～32wt％;MgO：4～7wt％;K2O+Na2O：＜0.3wt％;P2O5：0.01～0.1wt％;SO3：0.005～0.1wt％; in percentage by mass, wherein the total mass fraction of P 2O5 and SO 3 is 0.01-0.2 wt%;33wt% is less than CaO+MgO+10SO 3 is less than 38wt%. According to the invention, after the pulverized coal is introduced into P 2O5 and is matched with SO 3,SO3 and P 2O5 and the content is controlled within a certain range, the temperature range of melt fiber forming is increased, SO that the fiber content is increased, and the content of non-fiber substances in the fibers is reduced. The invention also provides a preparation method of the soluble ceramic fiber.
Description
Technical Field
The invention belongs to the technical field of inorganic fibers, and particularly relates to a soluble ceramic fiber and a preparation method thereof.
Background
The soluble fiber is fiber with low biological durability, which is soluble in physiological fluid after entering human body, so that the fiber has short residence time in human body, can be gradually decomposed by human body fluid and is discharged out of the body. The soluble fiber may be further processed as a major or minor component into a variety of articles including boards, mats, papers, carpets/felts, cottons/felts, shaped/formed articles, coating materials, amorphous compositions, and the like.
Existing soluble fibers include soluble ceramic fibers, soluble glass fibers, soluble basalt fibers, and the like.
In the preparation process of the existing soluble ceramic fiber, the problems of difficult melt melting, poor fiber diameter stability, non-centralized size distribution, high non-fibrous substance content in the fiber forming process and the like exist.
Disclosure of Invention
The invention aims to provide a soluble ceramic fiber and a preparation method thereof, wherein the soluble ceramic fiber has good diameter stability and low non-fibrous substance content.
The invention provides a soluble ceramic fiber which comprises the following components in percentage by mass:
SiO2：62～68wt％；
Al2O3：＜3wt％；
CaO：25～32wt％；
MgO：4～7wt％；
K2O+Na2O：＜0.3wt％
P2O5：0.01～0.1wt％
SO3：0.005～0.1wt％
wherein the total mass fraction of P 2O5 and SO 3 is 0.02-0.15 wt%; the total mass fraction of CaO, mgO and 10SO 3 is more than 33wt% and less than 38wt%.
Preferably, in the soluble ceramic fiber, the molar ratio of O to Si is 2.2 to 3.5.
Preferably, in the soluble ceramic fiber, the fiber with the diameter of 1-2 μm accounts for 10-0 wt%, the fiber with the diameter of 2-3 μm accounts for 60-80 wt%, and the fiber with the diameter of 3`4 μm accounts for 10-20 wt%.
The present invention provides a method of preparing a soluble ceramic fiber as described above, comprising the steps of:
Mixing a silicon source, a magnesium source, a calcium source, alumina and pulverized coal, melting, spinning to form fibers, collecting cotton and needling to obtain the soluble ceramic fibers.
Preferably, the melting temperature is 1720 to 1800 ℃.
Preferably, the temperature of the spun yarn fiber forming is 1400-1600 ℃; the linear speed of the spinning and fiber forming is 150-180 m/s.
Preferably, the density of the pulverized coal is 1.4-1.6 g/cm 3, the granularity of the pulverized coal is 0.8-1.6 mm, the total sulfur content is less than or equal to 0.5%, and the phosphorus content is less than or equal to 0.2%.
Preferably, the silicon source is silica or quartz sand containing SiO 2;
The magnesium source is one or more of MgO-containing fused magnesia, light burned dolomite, heavy burned dolomite and forsterite;
the calcium source is one or more of lime containing CaO, light-burned dolomite, heavy-burned dolomite and wollastonite.
The invention provides a soluble ceramic fiber, which comprises the following components ：SiO2：62～68wt％;Al2O3：＜3wt％;CaO：25～32wt％;MgO：4～7wt％;K2O+Na2O：＜0.3wt％;P2O5：0.01～0.1wt％;SO3：0.005～0.1wt％; in percentage by mass, wherein the total mass fraction of P 2O5 and SO 3 is 0.01-0.2 wt%; the total mass fraction of CaO, mgO and SO 3 is more than 33wt% and less than 38wt%. According to the invention, after the pulverized coal is introduced into P 2O5 and is matched with SO 3,SO3 and P 2O5 and the content is controlled within a certain range, the temperature range of melt fiber forming is increased, SO that the fiber content is increased, and the content of non-fiber substances in the fibers is reduced. Meanwhile, the contents of P 2O5+SO3 and CaO+MgO need to be regulated and controlled, so that the line shrinkage in the use process is reduced.
Detailed Description
The invention provides a soluble ceramic fiber which comprises the following components in percentage by mass:
SiO2：62～68wt％；
Al2O3：＜3wt％；
CaO：25～32wt％；
MgO：4～7wt％；
K2O+Na2O：＜0.3wt％
P2O5：0.01～0.1wt％
SO3：0.005～0.1wt％
Wherein the total mass fraction of P 2O5 and SO 3 is 0.02-0.15 wt%; the total mass fraction of CaO, mgO and SO 3 is more than 33wt% and less than 38wt%.
In the present invention, the mass fraction of SiO 2 is preferably 62 to 68% by weight, such as 62% by weight, 63% by weight, 64% by weight, 65% by weight, 66% by weight, 67% by weight, 68% by weight, preferably a range value having any of the above values as an upper limit or a lower limit.
The mass fraction of Al 2O3 is preferably < 3 wt.%, more preferably < 1 wt.%.
The mass fraction of CaO is preferably 25 to 32% by weight, such as 25% by weight, 26% by weight, 27% by weight, 28% by weight, 29% by weight, 30% by weight, 31% by weight, 32% by weight, and preferably a range having any of the above values as an upper limit or a lower limit.
The mass fraction of MgO is preferably 4 to 7wt%, such as 4wt%,5wt%,6wt%,7wt%, and preferably a range having any of the above values as an upper limit or a lower limit.
The mass fraction of P 2O5 is preferably 0.01 to 0.1wt%, more preferably 0.02 to 0.08wt%, such as 0.01wt%,0.02wt%,0.03wt%,0.04wt%,0.05wt%,0.06wt%,0.07wt%,0.08wt%,0.09wt%,0.1wt%, preferably a range having any of the above values as an upper limit or a lower limit.
The mass fraction of SO 3 is preferably 0.005 to 0.1wt%, more preferably 0.01 to 0.08wt%, such as 0.005wt%,0.01wt%,0.02wt%,0.03wt%,0.04wt%,0.05wt%,0.06wt%,0.07wt%,0.08wt%,0.09wt%,0.1wt%, preferably a range having any of the above values as an upper limit or a lower limit.
In the invention, SO 3 and P 2O5 are mainly introduced by pulverized coal, and SO 3 and P 2O5 are introduced SO as to reduce the melting temperature on one hand and enable the pulverized coal to be melted under the condition of lower than the conventional melting temperature of 1800-2000 ℃; and the contents of SO 3 and P 2O5 are controlled within a certain range, SO that SO 3 has the defect of reducing the strength of the fiber for the conventional soluble fiber, but after the SO 3 is matched with P 2O5 and the content is controlled within a certain range, the temperature range of melt fiber forming is increased, SO that the fiber content is increased, and the content of non-fiber substances in the fiber is reduced. The proportion of non-fibrous material in the soluble ceramic fibers in the invention is 25-35wt%. (wherein the non-fibrous material comprises dust having an average particle size of < 45 μm, particles having an average particle size of 45-212 μm, and shot having an average particle size of > 212 μm).
In the present invention, the total mass fraction of P 2O5 and SO 3 is preferably 0.02 to 0.15wt%, more preferably 0.05 to 0.12wt%, and for example 0.02wt％、0.03wt％、0.04wt％、0.05wt％、0.06wt％、0.07wt％、0.08wt％、0.09wt％、0.1wt％、0.11wt％、0.12wt％、0.13wt％、0.14wt％、0.15wt％,, is preferably a range having any of the above values as an upper limit or a lower limit.
In the present invention, the O/Si molar ratio in the soluble ceramic fiber is controlled to be in the range of 2.2 to 3.5, preferably 2.5 to 3.3. The diameter change of the fiber in the fiber forming process can be controlled in the proportion, and the diameter stability of the fiber in the fiber forming process is improved. The fiber product can not be manufactured in the following processing procedures such as needling technology, etc. because the O/Si molar ratio is too high, fiber formation can not be realized, the fiber diameter of the formed fiber is larger, and the fiber is unevenly distributed.
In the present invention, 33 wt.% < CaO+MgO+10SO 3 < 38 wt.%, preferably 33 wt.% < CaO+MgO+10SO 3 < 35 wt.%. In the present invention, "10SO 3" means 10 times the mass fraction of SO 3.
The invention also provides a preparation method of the soluble ceramic fiber, which comprises the following steps:
Mixing a silicon source, a magnesium source, a calcium source, alumina and pulverized coal, melting, spinning to form fibers, collecting cotton and needling to obtain the soluble ceramic fibers.
In the invention, the silicon source is silica or quartz sand containing SiO 2; the magnesium source is one or more of MgO-containing fused magnesia, light burned dolomite, heavy burned dolomite and forsterite; the calcium source is one or more of lime containing CaO, light calcined dolomite, heavy calcined dolomite and wollastonite; the density of the pulverized coal is 1.4-1.6 g/cm 3, the granularity of the pulverized coal is 0.8-1.6 mm, the total sulfur content is less than or equal to 0.5%, and the phosphorus content is less than or equal to 0.2%.
In the present invention, the relation of the amounts of the silicon source, the magnesium source, the calcium source, the alumina and the pulverized coal can be adjusted accordingly according to the above-described composition of the soluble ceramic fiber.
In the present invention, the melting temperature is preferably 1720 to 1800 ℃, more preferably 1750 to 1760 ℃, such as 1720 ℃,1730 ℃,1740 ℃,1750 ℃,1760 ℃,1770 ℃,1780 ℃,1790 ℃,1800 ℃, preferably in a range of any of the above values as an upper or lower limit.
In the present invention, the temperature of the spun yarn forming is preferably 1400 to 1600 ℃, more preferably 1540 to 1560 ℃, such as 1400 ℃,1420 ℃,1440 ℃,1460 ℃,1480 ℃,1500 ℃,1520 ℃,1540 ℃,1560 ℃,1580 ℃,1600 ℃, preferably a range value with any of the above values as an upper limit or a lower limit; the linear velocity of the spun yarn fiber is preferably 150 to 180m/s, more preferably 160 to 170m/s.
The apparatus used for melting and fiberizing is not particularly limited in the present invention, and preferably, the apparatus described in patent ZL201921802736.5 and ZL201920795574.0 can be used.
After the silk is spun into fibers, cotton is collected, and fiber aggregates formed by the cotton collection continuously enter a needling machine to be needled, so that the soluble ceramic fibers are obtained.
The fiber aggregate of the soluble ceramic fiber prepared by the conventional proportion and method comprises 20-30wt% of fiber with the diameter of 1-2 mu m, 50-60wt% of fiber with the diameter of 2-3 mu m and 10-20wt% of fiber with the diameter of 3-4 mu m. Wherein, the excessive fiber proportion of the diameter of 1-2 mu m leads to larger dust, and the fiber proportion of 2-3 mu m is too small, so the heat conductivity coefficient is higher. In the soluble ceramic fiber prepared according to the formula and the method of the invention, the fiber with the diameter of 1-2 μm accounts for 10-20wt% of the fiber aggregate, the fiber with the diameter of 2-3 μm accounts for 60-80wt% of the fiber aggregate, and the fiber with the diameter of 3-4 μm accounts for 10-20wt% of the fiber aggregate.
The biological solubility of the fiber aggregate ranges from 198 mg/L to 240mg/L; the fiber aggregate has a line shrinkage in the use process of less than or equal to 2% at 1100 ℃ for 24 hours.
The soluble ceramic fibers of the present invention are used in a basic or neutral alkaline atmosphere (pH > 7).
The invention provides a soluble ceramic fiber, which comprises the following components ：SiO2：62～68wt％;Al2O3：＜3wt％;CaO：25～32wt％;MgO：4～7wt％;K2O+Na2O：＜0.3wt％;P2O5：0.01～0.1wt％;SO3：0.005～0.1wt％; in percentage by mass, wherein the total mass fraction of P 2O5 and SO 3 is 0.01-0.2 wt%; the total mass fraction of CaO, mgO and SO 3 is more than 33wt% and less than 38wt%. According to the invention, after the pulverized coal is introduced into P 2O5 and is matched with SO 3,SO3 and P 2O5 and the content is controlled within a certain range, the temperature range of melt fiber forming is increased, SO that the fiber content is increased, and the content of non-fiber substances in the fibers is reduced. Meanwhile, the contents of P 2O5+SO3 and CaO+MgO need to be regulated and controlled, so that the line shrinkage in the use process is reduced.
In order to further illustrate the present invention, the following examples are provided to describe in detail a soluble ceramic fiber and a method for preparing the same, but should not be construed to limit the scope of the present invention.
Examples 1 to 7 and comparative examples 1 to 27
According to the proportioning requirements in Table 1, the required raw materials of wollastonite powder, silicon dioxide, magnesia, alumina and coal dust are uniformly mixed according to different proportions, are continuously melted at 1720-1780 ℃ to form fibers by spinning, the fiber forming temperature is 1540-1560 ℃, the spinning speed is 160m/s, and cotton blanks formed by collecting cotton continuously enter a needling machine to be needled and formed, so that the soluble ceramic fibers are obtained.
Table 1 composition (wt%) of soluble fiber prepared in examples and comparative examples
Table 2 results of property measurements of the products in examples and comparative examples
As is clear from tables 1 and 2, the soluble ceramic fibers of examples 1 to 6 of the present invention have significantly improved properties such as non-fibrous material content, solubility and diameter stability, as compared with the soluble ceramic fibers of comparative examples 1 to 27.
The foregoing is merely a preferred embodiment of the present invention and it should be noted that modifications and adaptations to those skilled in the art may be made without departing from the principles of the present invention, which are intended to be comprehended within the scope of the present invention.
Claims (8)
1. A soluble ceramic fiber comprising the following components in mass fraction:
SiO2：62～68wt％；
Al2O3：＜3wt％；
CaO：25～32wt％；
MgO：4～7wt％；
K2O+Na2O：＜0.3wt％
P2O5：0.01～0.1wt％
SO3：0.005～0.1wt％
Wherein the total mass fraction of P 2O5 and SO 3 is 0.02-0.15 wt%;33wt% is less than CaO+MgO+10SO 3 is less than 38wt%.
2. The soluble ceramic fiber according to claim 1, wherein the molar ratio of O to Si in the soluble ceramic fiber is 2.2 to 3.5.
3. The soluble ceramic fiber according to claim 2, wherein the soluble ceramic fiber has a fiber ratio of 1 to 2 μm of 10 to 0wt%, a fiber ratio of 2 to 3 μm of 60 to 80wt%, and a fiber ratio of 3`4 μm of 10 to 20wt%.
4. A method of preparing the soluble ceramic fiber of claim 1, comprising the steps of:
Mixing a silicon source, a magnesium source, a calcium source, alumina and pulverized coal, melting, spinning to form fibers, collecting cotton and needling to obtain the soluble ceramic fibers.
5. The method according to claim 4, wherein the melting temperature is 1720℃to 1800 ℃.
6. The method according to claim 4, wherein the temperature of the spun yarn fiber is 1400-1600 ℃; the linear speed of the spinning and fiber forming is 150-180 m/s.
7. The method according to any one of claims 4 to 6, wherein the pulverized coal has a density of 1.4 to 1.6g/cm 3, a pulverized coal particle size of 0.8 to 1.6mm, a total sulfur content of 0.5% or less, and a phosphorus content of 0.2% or less.
8. The method of claim 7, wherein the silicon source is silica or quartz sand containing SiO 2;
The magnesium source is one or more of MgO-containing fused magnesia, light burned dolomite, heavy burned dolomite and forsterite;
the calcium source is one or more of lime containing CaO, light-burned dolomite, heavy-burned dolomite and wollastonite.
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| CN202410078765.0A CN117888235A (en) | 2024-01-19 | 2024-01-19 | Soluble ceramic fiber and preparation method thereof |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202410078765.0A CN117888235A (en) | 2024-01-19 | 2024-01-19 | Soluble ceramic fiber and preparation method thereof |
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| CN117888235A true CN117888235A (en) | 2024-04-16 |
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