CN104695054A - Rapid and continuous preparation method of fire-resistant fiber - Google Patents
Rapid and continuous preparation method of fire-resistant fiber Download PDFInfo
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- CN104695054A CN104695054A CN201310660327.7A CN201310660327A CN104695054A CN 104695054 A CN104695054 A CN 104695054A CN 201310660327 A CN201310660327 A CN 201310660327A CN 104695054 A CN104695054 A CN 104695054A
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Abstract
The invention relates to a rapid and continuous preparation method of fire-resistant fiber, belonging to the field of spinning. The rapid and continuous preparation method of fire-resistant fiber comprises the following steps: pulping, spinning and thermal treatment, wherein the thermal treatment step comprises the following steps: placing the raw silks obtained by spinning into a sintering furnace at atmospheric pressure, firstly increasing the temperature to 1430-1480DEG C at the speed of 60-80DEG C/min, preserving the temperature for 0.2-0.5h, then increasing the temperature to 1510-1570DEG C at the speed of 5-20DEG C/min, and preserving the temperature for 0.2-2h. The method utilizes the characteristics of mullite crystal form transformation, the time for obtaining high-quality mullite fibers can be greatly shortened even under two-step sintering, and the rapid continuous sintering can be realized.
Description
Technical field
The present invention relates to a kind of quick continuous production method of refractory fibre, belong to spinning field.
Background technology
Mullite fiber is a kind of refractory material of high-quality, it has features such as expanding evenly, thermal shock resistance is fabulous, load softening point is high, high-temerature creep value is little, hardness is large, resistance to chemical corrosion is good, and its weaving techniques mainly comprises sol-gal process, polymerization, melt blending spin processes etc.
When carrying out melt blending weaving mullite fiber, for ensureing the surface flatness of gained fiber and forming the fiber of mullite crystal formation, the sintering in later stage need carry out under vacuo and need ensure longer sintering time.。
Summary of the invention
The object of this invention is to provide a kind of quick continuous production method of refractory fibre, utilize the method to prepare sintering time short and carry out without the need under vacuum again.
A kind of quick continuous production method of refractory fibre, comprising heat treatment step described in slurrying, spinning and heat treated step is: under normal pressure, spinning gained precursor is placed in sintering furnace, first 1430 DEG C ~ 1480 DEG C are warming up to the speed of 60 ~ 80 DEG C/min, after insulation 0.2 ~ 0.5h, 1510 DEG C ~ 1570 DEG C are warming up to, insulation 0.2 ~ 2h with the speed of 5 ~ 20 DEG C/min.
The preferred described heat treatment step of quick continuous production method of refractory fibre of the present invention is: under normal pressure, spinning gained precursor is placed in sintering furnace, first 1450 DEG C ~ 1470 DEG C are warming up to the speed of 60 ~ 80 DEG C/min, after insulation 0.2 ~ 0.3h, 1530 DEG C ~ 1550 DEG C are warming up to, insulation 0.2 ~ 0.5h with the speed of 5 ~ 10 DEG C/min.
The step of the preferred described slurrying of quick continuous production method of refractory fibre of the present invention is: by Al
2o
3with SiO
2material powder in molar ratio 3:2.05 ~ 2.25 is dissolved in mixed solution, stirs,
Wherein, described Al
2o
3with SiO
2the average grain diameter of material powder is all at 1 μm ~ 100 μm; Described mixed solution is the solution that PVA, PVB and diluent form, and wherein PVA and PVB accounts for the weight ratio of 10 ~ 35%, PVA and PVB of mixed solution gross weight is 1:2 ~ 10.
The preferred described pulping stage of quick continuous production method of refractory fibre of the present invention is: by Al
2o
3with SiO
2material powder in molar ratio 3:2.12 ~ 2.20 is dissolved in solution, stirs.
In the step of the preferred described slurrying of quick continuous production method of refractory fibre of the present invention, described Al
2o
3with SiO
2the average grain diameter of material powder is all at 10 μm ~ 50 μm.
In the step of the preferred described slurrying of quick continuous production method of refractory fibre of the present invention, PVA and PVB accounts for 15 ~ 20% of mixed solution gross weight.
In the step of the preferred described slurrying of quick continuous production method of refractory fibre of the present invention, the weight ratio of PVA and PVB is 1:3 ~ 5.
The preferred described diluent of quick continuous production method of refractory fibre of the present invention is ethanol or propyl alcohol.
The preferred described spinning process of quick continuous production method of refractory fibre of the present invention is: slurrying gained slurries are placed in device for spinning, are heated to 100 DEG C ~ 200 DEG C, and insulation 0.5 ~ 1h, carries out spinning with the speed of 20 ~ 400m/min subsequently, obtain precursor.
The present invention's preferred technical scheme is:
1. slurrying: by Al
2o
3with SiO
2material powder in molar ratio 3:2.05 ~ 2.25 is dissolved in mixed solution, stirs,
Wherein, described Al
2o
3with SiO
2the average grain diameter of material powder is all at 1 μm ~ 100 μm; Described mixed solution is the solution that PVA, PVB and diluent form, and wherein PVA and PVB accounts for the weight ratio of 10 ~ 35%, PVA and PVB of mixed solution gross weight is 1:2 ~ 10;
2. spinning: slurrying gained slurries are placed in device for spinning, is heated to 100 DEG C ~ 200 DEG C, and insulation 0.5 ~ 1h, carries out spinning with the speed of 20 ~ 400m/min subsequently, obtain precursor.
3. heat treatment: under normal pressure, is placed in sintering furnace by spinning gained precursor, is first warming up to 1430 DEG C ~ 1480 DEG C with the speed of 60 ~ 80 DEG C/min, after insulation 0.2 ~ 0.5h, is warming up to 1510 DEG C ~ 1570 DEG C with the speed of 5 ~ 20 DEG C/min, insulation 0.2 ~ 2h.
The invention has the beneficial effects as follows: the preparation method of mullite fiber of the present invention, the sintering step of the method comprises two steps, its objective is and mullite was changed fully two crystal transfer stages, ensure mullite sufficient nucleation at first step heat treatment stages; Second stage heat treatment makes mullite nucleus obtain good growth, though be two heat treatment stages, but due to transformation of crystal abundant, therefore, shorten the time obtaining high-quality mullite fiber, realize quick continuous sintering.In addition, with the mixed solution of PVA and PVB for additive, adopt melt spinning method to carry out spinning, effectively improve the volatilization situation of additive, reduce the surface roughness of gained fiber.Meanwhile, due to the pulp furnish having selected silica excessive, raw materials used granularity is declined, has saved production cost.
Detailed description of the invention
Following non-limiting example can make the present invention of those of ordinary skill in the art's comprehend, but does not limit the present invention in any way.
Embodiment 1
1. slurrying: by Al
2o
3with SiO
2material powder in molar ratio 3:2.10 is dissolved in mixed solution, stirs,
Wherein, described Al
2o
3with SiO
2the average grain diameter of material powder is all at 20 μm; Described mixed solution is the solution that PVA, PVB and propyl alcohol form, and wherein PVA and PVB accounts for the weight ratio of 20%, PVA and PVB of mixed solution gross weight is 1:4;
2. spinning: slurrying gained slurries are placed in device for spinning, are heated to 120 DEG C, insulation 1h, carries out spinning with the speed of 50m/min subsequently, obtains precursor.
3. heat treatment: under normal pressure, is placed in sintering furnace by spinning gained precursor, is first warming up to 1460 DEG C with the speed of 80 DEG C/min, after insulation 0.3h, is warming up to 1540 DEG C with the speed of 5 DEG C/min, insulation 0.5h.
Gained fiber is even, surface smoothing, and diameter is 45 μm.
Embodiment 2
1. slurrying: by Al
2o
3with SiO
2material powder in molar ratio 3:2.25 is dissolved in mixed solution, stirs,
Wherein, described Al
2o
3with SiO
2the average grain diameter of material powder is all at 20 μm; Described mixed solution is the solution that PVA, PVB and ethanol form, and wherein PVA and PVB accounts for the weight ratio of 16%, PVA and PVB of mixed solution gross weight is 1:5;
2. spinning: slurrying gained slurries are placed in device for spinning, are heated to 120 DEG C, insulation 1h, carries out spinning with the speed of 50m/min subsequently, obtains precursor.
3. heat treatment: under normal pressure, is placed in sintering furnace by spinning gained precursor, is first warming up to 1440 DEG C with the speed of 70 DEG C/min, after insulation 0.35h, is warming up to 1570 DEG C with the speed of 10 DEG C/min, insulation 0.5h.
Gained fiber is even, surface smoothing, and diameter is 27 μm.
Claims (9)
1. the quick continuous production method of a refractory fibre, comprise slurrying, spinning and heat treated step, it is characterized in that: described heat treatment step is: under normal pressure, spinning gained precursor is placed in sintering furnace, first 1430 DEG C ~ 1480 DEG C are warming up to the speed of 60 ~ 80 DEG C/min, after insulation 0.2 ~ 0.5h, be warming up to 1510 DEG C ~ 1570 DEG C with the speed of 5 ~ 20 DEG C/min, insulation 0.2 ~ 2h.
2. method according to claim 1, it is characterized in that: described heat treatment step is: under normal pressure, spinning gained precursor is placed in sintering furnace, first 1450 DEG C ~ 1470 DEG C are warming up to the speed of 60 ~ 80 DEG C/min, after insulation 0.2 ~ 0.3h, 1530 DEG C ~ 1550 DEG C are warming up to, insulation 0.2 ~ 0.5h with the speed of 5 ~ 10 DEG C/min.
3. method according to claim 1, is characterized in that: the step of described slurrying is: by Al
2o
3with SiO
2material powder in molar ratio 3:2.05 ~ 2.25 is dissolved in mixed solution, stirs,
Wherein, described Al
2o
3with SiO
2the average grain diameter of material powder is all at 1 μm ~ 100 μm; Described mixed solution is the solution that PVA, PVB and diluent form, and wherein PVA and PVB accounts for the weight ratio of 10 ~ 35%, PVA and PVB of mixed solution gross weight is 1:2 ~ 10.
4. method according to claim 3, is characterized in that: described pulping stage is: by Al
2o
3with SiO
2material powder in molar ratio 3:2.12 ~ 2.20 is dissolved in solution, stirs.
5. method according to claim 3, is characterized in that: in the step of described slurrying, described Al
2o
3with SiO
2the average grain diameter of material powder is all at 10 μm ~ 50 μm.
6. method according to claim 3, is characterized in that: in the step of described slurrying, and PVA and PVB accounts for 15 ~ 20% of mixed solution gross weight.
7. method according to claim 3, is characterized in that: in the step of described slurrying, and the weight ratio of PVA and PVB is 1:3 ~ 5.
8. method according to claim 3, is characterized in that: described diluent is ethanol or propyl alcohol.
9. method according to claim 1, is characterized in that: described spinning process is: slurrying gained slurries are placed in device for spinning, is heated to 100 DEG C ~ 200 DEG C, and insulation 0.5 ~ 1h, carries out spinning with the speed of 20 ~ 400m/min subsequently, obtain precursor.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310660327.7A CN104695054A (en) | 2013-12-05 | 2013-12-05 | Rapid and continuous preparation method of fire-resistant fiber |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310660327.7A CN104695054A (en) | 2013-12-05 | 2013-12-05 | Rapid and continuous preparation method of fire-resistant fiber |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN104695054A true CN104695054A (en) | 2015-06-10 |
Family
ID=53342580
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201310660327.7A Pending CN104695054A (en) | 2013-12-05 | 2013-12-05 | Rapid and continuous preparation method of fire-resistant fiber |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN104695054A (en) |
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2013
- 2013-12-05 CN CN201310660327.7A patent/CN104695054A/en active Pending
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| PB01 | Publication | ||
| WD01 | Invention patent application deemed withdrawn after publication |
Application publication date: 20150610 |