CN102718495B - Magnesium silicon ceramic fiber and preparation method thereof - Google Patents

Abstract

The invention relates to a magnesium-silicon ceramic fiber and a preparation method thereof. The technical scheme is: first use 1~10wt% waste marble powder, 15~40wt% forsterite powder, 2~8wt% albite powder or potassium feldspar powder, 40~70wt% quartz sand powder and 1~3wt% % industrial sodium tripolyphosphate as raw materials, pressed into green bodies, heat treated at 1000~1300°C for 60~90min; then crushed, ground to 120 mesh, plus 1~5wt% industrial magnesium chloride and 0.5~3wt% raw materials % industrial starch, mixed evenly; then put the evenly mixed material in a resistance furnace, heat up to 1500~1700°C, and spin the silk directly after melting to obtain ceramic fibers; finally, heat treat the ceramic fibers at 600~900°C for 1 ~ 4 hours, the magnesium-silicon ceramic fiber is obtained. The invention has the characteristics of low melting temperature, easy operation of fiber forming process and low production cost; the prepared product has smooth surface, high mechanical strength, high service temperature and high biodegradation rate.

Description

A kind of magnesium silicon ceramic fiber and preparation method thereof

technical field

The invention belongs to the technical field of ceramic fibers. It specifically relates to a magnesium-silicon ceramic fiber and a preparation method thereof.

Background technique

The fine dust particles produced during the production, use and post-use disassembly of traditional aluminum silicate ceramic fibers are difficult to be degraded by human body fluids after being inhaled into the respiratory system by the human body, which will induce inflammation of the respiratory system and even canceration. Waste aluminum silicate fibers that have lost their usability are usually disposed of by landfill or other methods. Due to their stable chemical properties, they are difficult to be degraded and will also pollute the environment. Therefore, the International Association for Research on Cancer classifies aluminum silicate ceramic fibers as possible carcinogens. Researchers at home and abroad have successively researched and developed a series of products of soluble ceramic fibers, such as magnesium-silicon ceramic fibers. Magnesium-silicon ceramic fibers are usually prepared by blowing or spinning after the raw materials are melted at high temperature; the existence of a high content of magnesium oxide in the fiber composition makes it have a high biodegradation rate in human body fluids; The presence of higher content of silica and magnesium oxide in the fiber composition makes the fiber have a higher service temperature. However, there are still some deficiencies in the preparation and performance of the current magnesium-silicon ceramic fibers. For example, limited by the composition characteristics, the melting temperature range of the raw materials is relatively high, the high-temperature melt viscosity is high, and the viscosity change rate during the fiber forming process is not easy to control, so the fiber forming operation process is more difficult; Crystallization and pulverization occur, which in turn leads to a reduction in the service life of the fiber.

In addition, natural marble produces a lot of waste during the processing process: stone scraps and stone powder. At present, stone leftovers have been fully reused, but there is no better treatment method for stone powder, and it can only be piled up. Simple stacking treatment not only wastes land and resources, but also pollutes water sources and local air quality. Therefore, it is of great significance to properly handle and utilize these stone powder wastes for rational development of resources.

At present, in order to solve the problem of difficult fiber formation of magnesia-silicon ceramic fibers in production, zirconia, titanium oxide or rare earth metal oxides are usually introduced into the composition, but this brings about the reduction of other properties of the fiber, such as the fiber diameter is too large. Large or too small, reduced mechanical strength, increased high-temperature line shrinkage, reduced biodegradation rate, etc.

In short, there are still some deficiencies in the preparation technology of magnesium-silicon ceramic fibers: high production cost, high melting temperature of raw materials, difficult operation of fiber-forming process and fiber performance need to be improved.

Contents of the invention

The invention aims to overcome the disadvantages of the prior art, and aims to provide a preparation method of magnesium-silicon ceramic fiber with low production cost, low melting temperature and easy operation of the fiber-forming process. The magnesia-silicon ceramic fiber prepared by the method has relatively high service temperature and high biodegradation rate.

In order to achieve the above object, the technical scheme adopted in the present invention is:

First use 1~10wt% waste marble powder, 15~40wt% forsterite powder, 2~8wt% albite or potassium feldspar powder, 40~70wt% quartz sand powder and 1~3wt% industrial tripolymer Sodium phosphate is mixed as raw material, pressed into green body, heat treated at 1000~1300℃ for 60~90min;

Then the heat-treated material is crushed, ground to 120 mesh, and the industrial magnesium chloride of 1-5wt% and 0.5-3wt% of the raw material are added, and mixed uniformly;

Then place the uniformly mixed material in a resistance furnace, raise the temperature to 1500~1700°C, spin the filaments directly after melting, and obtain ceramic fibers;

Finally, the ceramic fiber is heat-treated at 600-900°C for 1-4 hours to obtain the magnesium-silicon ceramic fiber.

In the above technical scheme:

The particle size of the waste marble powder is 80-120 mesh, and the _CaCO3 content is greater than 50wt%;

The particle size of forsterite powder is 40~120 mesh; its main chemical composition is: SiO ₂ is 25~35wt%, MgO is 50~65wt%, CaO is 0.5~2wt%, Fe ₂ O ₃ is less than 8wt%;

The particle size of quartz sand powder is 40~120 mesh; its main chemical composition is: SiO ₂ is 90~99wt%, Fe ₂ O ₃ is less than 0.05wt%;

The particle size of albite powder is 40~120 mesh; its main chemical composition is: SiO ₂ is 63~70wt%, Al ₂ O ₃ is 16~25wt%, Na ₂ O is 9~15wt%;

The particle size of potassium feldspar powder is 40~120 mesh; its main chemical composition is: SiO ₂ is 64~69wt%, Al ₂ O ₃ is 16~23wt%, K ₂ O is 9~18wt%;

The particle size of industrial sodium tripolyphosphate is 80~120 mesh; the content of Na ₅ P ₃ O ₁₀ is greater than 90wt%;

The particle size of industrial magnesium chloride is 80 ~ 120 mesh; wherein MgCl ₂ content is greater than 40wt%;

The pressing pressure is 35~45MPa.

Owing to adopting above-mentioned technical scheme, the present invention has following positive effect compared with prior art:

1. The melting temperature of the present invention is low, the viscosity of the melt in the fiber-forming range changes smoothly, and the fiber-forming process is easy to control;

2, the raw material price that the present invention adopts is cheap, and production cost is low, has very big industrialization prospect;

3. The magnesium-silicon ceramic fiber prepared by the present invention has smooth surface, high mechanical strength, service temperature greater than 1200°C, and biodegradation rate greater than 150ng/(cm ² ·h).

Therefore, the invention has the characteristics of low melting temperature, easy operation of the fiber forming process and low production cost; the prepared magnesium-silicon ceramic fiber has smooth surface, high mechanical strength, high service temperature and high biodegradation rate.

Detailed ways

The present invention will be further described below in combination with specific embodiments, which are not intended to limit the protection scope thereof.

In order to avoid duplication, first the raw materials of this specific embodiment are described as follows, and will not be repeated in each embodiment:

The particle size of the waste marble powder is 80-120 mesh, and the _CaCO3 content is greater than 50wt%;

The particle size of forsterite powder is 40~120 mesh; its main chemical composition is: SiO ₂ is 25~35wt%, MgO is 50~65wt%, CaO is 0.5~2wt%, Fe ₂ O ₃ is less than 8wt%;

The particle size of quartz sand powder is 40~120 mesh; its main chemical composition is: SiO ₂ is 90~99wt%, Fe ₂ O ₃ is less than 0.05wt%;

The particle size of albite powder is 40~120 mesh; its main chemical composition is: SiO ₂ is 63~70wt%, Al ₂ O ₃ is 16~25wt%, Na ₂ O is 9~15wt%;

The particle size of potassium feldspar powder is 40~120 mesh; its main chemical composition is: SiO ₂ is 64~69wt%, Al ₂ O ₃ is 16~23wt%, K ₂ O is 9~18wt%;

The particle size of industrial sodium tripolyphosphate is 80~120 mesh; the content of Na ₅ P ₃ O ₁₀ is greater than 90wt%;

The particle size of industrial magnesium chloride is 80 ~ 120 mesh; wherein MgCl ₂ content is greater than 40wt%;

The pressing pressure is 35~45MPa.

Example 1

A magnesium-silicon ceramic fiber and a preparation method thereof. First use 6~10wt% waste marble stone powder, 30~40wt% forsterite powder, 50~60wt% quartz sand powder, 2~5wt% potassium feldspar powder, 1~2wt% industrial sodium tripolyphosphate as raw materials Mix and press into green body, heat treatment at 1000~1150℃ for 60~90min;

Then the heat-treated material is crushed, ground to 120 mesh, and the industrial magnesium chloride of 1-3wt% and 0.5-1.5wt% of the raw material are added, and mixed uniformly;

Then place the uniformly mixed material in a resistance furnace, raise the temperature to 1500~1700°C, spin the filaments directly after melting, and obtain ceramic fibers;

Finally, the ceramic fiber is heat-treated at 800-900°C for 2-3 hours to obtain the magnesium-silicon ceramic fiber.

The magnesium-silicon ceramic fiber prepared in this example: the surface of the fiber is smooth, the mechanical strength is high, the service temperature is greater than 1200° C., and the biodegradation rate is greater than 150 ng/(cm ² ·h).

Example 2

A magnesium-silicon ceramic fiber and a preparation method thereof. First use 1~4wt% waste marble stone powder, 15~25wt% forsterite powder, 60~70wt% quartz sand powder, 4~8wt% albite powder, 2~3wt% industrial sodium tripolyphosphate as raw materials Mix and press into green body, heat treatment at 1100~1200℃ for 60~90min;

Then the heat-treated material is crushed and ground to 120 mesh, and the industrial magnesium chloride of 2 to 4wt% and the industrial starch of 1 to 2wt% of the raw materials are added, and mixed uniformly;

Then place the uniformly mixed material in a resistance furnace, raise the temperature to 1500~1700°C, spin the filaments directly after melting, and obtain ceramic fibers;

Finally, the ceramic fiber is heat-treated at 600-700°C for 3-4 hours to obtain the magnesium-silicon ceramic fiber.

The magnesium-silicon ceramic fiber prepared in this example: the surface of the fiber is smooth, the mechanical strength is high, the service temperature is greater than 1200° C., and the biodegradation rate is greater than 180 ng/(cm ² ·h).

Example 3

A magnesium-silicon ceramic fiber and a preparation method thereof. First use 3~7wt% waste marble powder, 22~30wt% forsterite powder, 56~65wt% quartz sand powder, 2~5wt% albite powder, 1~2wt% industrial sodium tripolyphosphate as raw materials Mix and press into green body, heat treatment at 1200~1300℃ for 60~90min;

Then the heat-treated material is crushed and ground to 120 orders, and the industrial magnesium chloride of 3 to 5wt% and the industrial starch of 2 to 3wt% of the raw materials are added, and mixed uniformly;

Then place the uniformly mixed material in a resistance furnace, raise the temperature to 1500~1700°C, spin the filaments directly after melting, and obtain ceramic fibers;

Finally, the ceramic fiber is heat-treated at 700-800°C for 1-2 hours to obtain the magnesium-silicon ceramic fiber.

The magnesium-silicon ceramic fiber prepared in this example has smooth fiber surface, high mechanical strength, a service temperature greater than 1200°C, and a biodegradation rate greater than 180ng/(cm ² ·h).

Example 4

A magnesium-silicon ceramic fiber and a preparation method thereof. First use 8~10wt% waste marble stone powder, 35~40wt% forsterite powder, 40~50wt% quartz sand powder, 4~8wt% potassium feldspar powder, 2~3wt% industrial sodium tripolyphosphate as raw materials Mix and press into green body, heat treatment at 1000~1100℃ for 60~90min;

Then the heat-treated material is crushed and ground to 120 mesh, and the industrial magnesium chloride of 1-2wt% and the industrial starch of 0.5-1wt% of the raw materials are added, and mixed uniformly;

Then place the uniformly mixed material in a resistance furnace, raise the temperature to 1500~1700°C, spin the filaments directly after melting, and obtain ceramic fibers;

Finally, the ceramic fiber is heat-treated at 600-700°C for 2-3 hours to obtain the magnesium-silicon ceramic fiber.

The magnesium-silicon ceramic fiber prepared in this example has smooth fiber surface, high mechanical strength, service temperature greater than 1200° C., and biodegradation rate greater than 200 ng/(cm ² ·h).

Example 5

A magnesium-silicon ceramic fiber and a preparation method thereof. First use 2~5wt% waste marble stone powder, 28~35wt% forsterite powder, 55~65wt% quartz sand powder, 3~6wt% potassium feldspar powder, 1~2wt% industrial sodium tripolyphosphate as raw materials Mix and press into green body, heat treatment at 1150~1250℃ for 60~90min;

Then the heat-treated material is crushed and ground to 120 orders, and the industrial magnesium chloride of 2 to 4wt% and the industrial starch of 2 to 3wt% of the raw materials are added, and mixed uniformly;

Then place the uniformly mixed material in a resistance furnace, raise the temperature to 1500~1700°C, spin the filaments directly after melting, and obtain ceramic fibers;

Finally, the ceramic fiber is heat-treated at 800-900°C for 2-3 hours to obtain the magnesium-silicon ceramic fiber.

The magnesium-silicon ceramic fiber prepared in this example has smooth fiber surface, high mechanical strength, service temperature greater than 1200° C., and biodegradation rate greater than 150 ng/(cm ² ·h).

Example 6

A magnesium-silicon ceramic fiber and a preparation method thereof. First use 7~9wt% waste marble powder, 30~40wt% forsterite powder, 45~55wt% quartz sand powder, 3~7wt% albite powder, 1~2wt% industrial sodium tripolyphosphate as raw materials Mix and press into green body, heat treatment at 1200~1300℃ for 60~90min;

Then the heat-treated material is crushed and ground to 120 mesh, and the industrial magnesium chloride of 4-5wt% and the industrial starch of 1-2wt% of the raw materials are added, and mixed uniformly;

Then place the uniformly mixed material in a resistance furnace, raise the temperature to 1500~1700°C, spin the filaments directly after melting, and obtain ceramic fibers;

Finally, the ceramic fiber is heat-treated at 700-800°C for 3-4 hours to obtain the magnesium-silicon ceramic fiber.

The magnesium-silicon ceramic fiber prepared in this example has smooth fiber surface, high mechanical strength, service temperature greater than 1200° C., and biodegradation rate greater than 200 ng/(cm ² ·h).

Compared with the prior art, this specific embodiment has the following positive effects:

1. The melting temperature of this specific embodiment is low, the melt viscosity changes gently within the fiber-forming range, and the fiber-forming process is easy to control;

2. The raw materials used in this specific embodiment are cheap, the production cost is low, and there is great industrialization prospect;

3. The magnesium-silicon ceramic fiber prepared in this specific embodiment has a smooth surface and high mechanical strength. The use temperature is higher than 1200° C., and the biodegradation rate is higher than 150 ng/(cm ² ·h).

Therefore, this specific embodiment has the characteristics of low melting temperature, easy operation of fiber-forming process and low production cost; the prepared magnesium-silicon ceramic fiber has smooth surface, high mechanical strength, high service temperature and high biodegradation rate.

Claims (10)

1. a preparation method of magnesium-silicon ceramic fiber, is characterized in that earlier with the waste marble stone powder of 1～10wt%, the forsterite powder of 15～40wt%, the albite powder of 2～8wt% or potassium feldspar powder, 40～ 70wt% quartz sand powder and 1~3wt% industrial sodium tripolyphosphate are mixed as raw materials, pressed into a green body, and heat treated at 1000~1300°C for 60~90min; Then the heat-treated material is crushed, ground to 120 mesh, and the industrial magnesium chloride of 1-5wt% and 0.5-3wt% of the raw material are added, and mixed uniformly; Then place the uniformly mixed material in a resistance furnace, raise the temperature to 1500~1700°C, spin the filaments directly after melting, and obtain ceramic fibers; Finally, the ceramic fiber is heat-treated at 600-900°C for 1-4 hours to obtain the magnesium-silicon ceramic fiber. 2. The preparation method of magnesia-silicon ceramic fiber according to claim 1, characterized in that the particle size of the waste marble stone powder is 80-120 mesh, wherein the _CaCO3 content is greater than 50wt%. 3. The preparation method of magnesium-silicon ceramic fiber according to claim 1, characterized in that the particle size of the forsterite powder is 40~120 mesh; its main chemical composition is: _SiO2 is 25~35wt%, MgO is 50 ~65wt%, CaO is 0.5~2wt%, Fe ₂ O ₃ is less than 8wt%. 4. The preparation method of magnesium-silicon ceramic fiber according to claim 1, characterized in that the particle size of the quartz sand powder is 40-120 mesh; its main chemical composition is: _SiO2 is 90-99wt%, _{Fe2O 3} is less than 0.05wt%. 5. The preparation method of magnesium-silicon ceramic fiber according to claim 1, characterized in that the particle size of the albite powder is 40-120 mesh; its main chemical composition is: SiO ₂ is 63-70wt%, Al ₂ O ₃ is 16~25wt%, Na ₂ O is 9~15wt%. 6. The preparation method of magnesium-silicon ceramic fiber according to claim 1, characterized in that the particle size of the potassium feldspar powder is 40-120 mesh; its main chemical composition is: SiO ₂ is 64-69wt%, Al ₂ O ₃ is 16~23wt%, and K ₂ O is 9~18wt%. 7. The preparation method of magnesium-silicon ceramic fiber according to claim 1, characterized in that the particle size of the industrial sodium tripolyphosphate is 80-120 mesh; wherein the Na ₅ P ₃ O ₁₀ content is greater than 90wt%. 8. The preparation method of magnesium-silicon ceramic fiber according to claim 1, characterized in that the pressing pressure is 35-45MPa. 9. The preparation method of magnesium-silicon ceramic fiber according to claim 1, characterized in that the particle size of the industrial magnesium chloride is 80-120 mesh; wherein the _MgCl content is greater than 40wt%. 10. The magnesium-silicon ceramic fiber prepared by the preparation method of the magnesium-silicon ceramic fiber according to any one of claims 1-9.