Quantitative analysis method for spinnability of continuous basalt fiber raw material

Abstract

The invention discloses a continuous basalt fiber raw material spinnability quantitative analysis method, and belongs to the field of inorganic nonmetallic materials. The method comprises the following steps: heating and melting a basalt fiber raw material, and quenching in water to obtain a glass body; crushing the glass body to obtain glass powder; heating the glass powder, collecting a thermal signal by using a thermal analysis method in the heating process, and obtaining a glass transition temperature T1 and a crystallization starting temperature T2; and calculating a spinnability parameter H by combining the glass transition temperature T1, the crystallization starting temperature T2 and the complete melting temperature T3 of the raw material, and evaluating. According to the method, the glass powder is prepared by melting, water quenching and crushing the raw materials, and the key characteristic temperature in the heating process is tested by utilizing a thermal analysis technology, so that quantitative evaluation on spinnability parameters of the complex raw materials is realized, and the spinnability of the basalt fiber raw materials is further evaluated.

Description

Technical Field

[0001] This invention belongs to the field of inorganic non-metallic materials, and specifically relates to a quantitative analysis method for the spinnability of continuous basalt fiber raw materials. Background Technology

[0002] Basalt fiber is a high-strength, alkali-resistant, and heat-resistant high-tech fiber material with applications in civil engineering, marine engineering, and fireproofing and insulation. Currently, the raw material for manufacturing basalt fiber is mainly natural basalt ore. Basalt is a typical igneous rock, widely distributed on the Earth's surface, but suitable basalt ore for high-performance fiber production is concentrated and has limited reserves. Furthermore, the composition and physical properties of natural basalt ore are unstable, and its spinnability fluctuates, which is detrimental to fiber manufacturing. Currently, basalt fiber manufacturing is developing towards multi-component formulations and modified additives. In addition, large quantities of coal-based solid waste, metallurgical solid waste, and mining solid waste have compositions similar to natural basalt and are also potential spinning raw materials. The spinnability of the raw material determines whether fiber manufacturing can be achieved. For the aforementioned basalt fiber raw materials with diverse and complex compositions, how to use simple methods to assess their spinnability is an urgent problem to be solved. Traditional tests for the spinnability of raw materials require simultaneous measurement of the viscosity-temperature profile of the melt and the upper limit of crystallization temperature. Measuring these parameters necessitates specialized equipment, is complex, and presents significant testing challenges. Furthermore, the testing process is difficult to directly correlate with the actual spinning process. Therefore, this application is hereby submitted. Summary of the Invention

[0003] This invention aims to provide a quantitative analysis method for the spinnability of continuous basalt fiber raw materials. By melting, water quenching and crushing the raw materials to obtain glass powder, and using thermal analysis technology to test the key characteristic temperatures of the heating process, a quantitative assessment of the spinnability parameters of complex raw materials can be achieved, thereby evaluating the spinnability of basalt fiber raw materials.

[0004] To achieve the above-mentioned objectives, the technical solution of the present invention is as follows: This invention provides a method for quantitative analysis of the spinnability of continuous basalt fiber raw materials, comprising the following steps: S1: Basalt fiber raw material is heated and melted, and then quenched in water to obtain a glassy substance.

[0005] Optionally, the basalt fiber raw material includes one or more combinations of single basalt ore, artificial compounding materials, or solid waste.

[0006] In some preferred embodiments, the combination includes one or two combinations of basalt ore and artificial batching materials or solid waste.

[0007] In some preferred embodiments, the solid waste includes coal gasification ash.

[0008] Furthermore, the heating and melting process involves heating to 1500-1650℃ and holding at that temperature for 6-16 hours.

[0009] Both the fiber preparation process and the fiber product are melts or glassy substances. The applicant discovered that, possibly because raw materials such as basalt and gasification slag may contain crystals, melting the raw materials can yield a glassy substance that truly reflects spinnability.

[0010] S2: The glass body is crushed to obtain glass powder.

[0011] Furthermore, the particle size of the glass powder is 200-250 mesh. The particle size of the glass powder affects the measurement of the initial crystallization temperature; generally, the larger the particle size, the higher the initial crystallization temperature. In addition, particle size also affects the accuracy of the thermal signal. Therefore, a particle size of 200-250 mesh is preferred for the glass powder.

[0012] S3: The glass powder is heated, and during the heating process, thermal signals are collected using thermal analysis methods to obtain the glass transition temperature T1 and the initiation crystallization temperature T2.

[0013] Furthermore, the heating is to a temperature above 1200°C; furthermore, the heating rate is 5-20°C / min.

[0014] Optionally, the thermal analysis method includes differential scanning calorimetry (DSC) or differential thermal analysis (DTA). The characteristic temperature is measured in absolute temperature scale.

[0015] S4: Calculate the spinnability parameter H by combining the glass transition temperature T1, the initial crystallization temperature T2, and the complete melting temperature T3 of the raw material, and evaluate it.

[0016] Furthermore, the method for calculating the spinnability parameter H is as follows: H=(T2-T1) / T3, If H > 0.01, the raw material is spinnable; if H ≤ 0.01, the raw material is not spinnable.

[0017] Optionally, the complete melting temperature T3 is measured by a melting point apparatus or obtained by thermodynamic calculation.

[0018] Compared with the prior art, the present invention has the following beneficial effects: (1) Glass powder is obtained by melting, water quenching and crushing the raw materials. Then, the key characteristic temperature is taken during the heating process, and the spinnability is described by quantitative parameters, which facilitates the comparison of the properties of different raw materials. (2) It is applicable to the evaluation of the spinnability of various spinning raw materials and can screen various potential basalt fiber raw materials. (3) The test process is simple, the thermal signal is accurate, and the data results are highly repeatable. Spinability parameters can be obtained in one go using a characterization method. The method is simple and fast. Attached Figure Description

[0019] Figure 1 This is a photograph of basalt fiber obtained after spinnability analysis in Example 1 of the present invention. Detailed Implementation

[0020] The terminology used in the implementation section of this application is for the purpose of explaining specific embodiments of this application only, and is not intended to limit this application.

[0021] Example 1 (1) Basalt ore from Weixian County, Hebei Province was selected. Its composition is shown in Table 1. It was melted at 1550℃ for 8 h and then water-quenched to form a glassy substance. Table 1 Raw material composition of Example 1 (2) Crush the obtained glass and sieve it to select glass powder of 200-250 mesh; (3) The obtained glass powder was heated to 1200 ℃ at a rate of 10 ℃ / min using DSC to obtain the glass transition temperature (T1=922 K) and the crystallization start temperature (T2=940 K). (4) The melting temperature (T3 = 1481 K) was measured using a melting point apparatus, and the spinnability parameter (H = 0.012) was calculated. This basalt ore can be spun into basalt fiber. The basalt fiber actually produced using the raw materials in this embodiment is as follows: Figure 1 As shown.

[0022] Example 2 (1) Select the gasification slag from the Shell gasifier of Lu'an Chemical Group. Its composition is shown in Table 2. Melt it at 1600℃ for 12 h and quench it in water to form a glassy substance. Table 2 Raw material composition of Example 2 (2) Crush the obtained glass and sieve it to select glass powder of 200-250 mesh; (3) The obtained glass powder was heated to 1200 ℃ at a rate of 10 ℃ / min using DSC to obtain the glass transition temperature (T1=1013 K) and the crystallization initiation temperature (T2=1041 K). (4) The melting temperature (T3=1710 K) was calculated using thermodynamic software, and the spinnability parameter (H=0.016) was obtained. This basalt ore can be spun into basalt fiber.

[0023] Example 3 (1) Select coal gasification slag from Yulin Energy and Chemical Coal-Water Slurry Gasification Furnace. Its composition is shown in Table 3. Melt it at 1500℃ for 12 h and quench it in water to form a glassy body. Table 3 Raw material composition of Example 3 (2) Crush the obtained glass and sieve it to select glass powder of 200-250 mesh; (3) The obtained glass powder was heated to 1200 ℃ at a rate of 10 ℃ / min using DSC to obtain the glass transition temperature (T1=925 K) and the crystallization initiation temperature (T2=941 K). (4) The melting temperature (T3=1609 K) was measured using a melting point apparatus, and the spinnability parameter (H=0.010) was calculated. This coal gasification slag cannot be spun into basalt fiber.

[0024] Comparative Example 1 (1) Select the same dry powder gasification furnace coal gasification slag as in Implementation 2, crush it, and screen it to select 200-250 mesh powder; (2) The obtained powder was heated to 1200 ℃ at a rate of 10 ℃ / min using DSC to obtain the glass transition temperature (T1=1017 K) and the crystallization initiation temperature (T2=1028 K). (3) The melting temperature (T3=1719 K) was measured using a melting point apparatus, and the spinnability parameter (H=0.064) was calculated. It was predicted that this coal gasification slag could not be spun into basalt fiber, but this coal gasification slag was spinnable, so the prediction failed.

[0025] Comparative Example 2 (1) Select the same dry powder gasification furnace coal gasification slag as in Implementation 2, melt it at 1600 ℃ for 1 h, and water quench it into a glassy body; (2) Crush the obtained glass and sieve it to select glass powder of 200-250 mesh; (3) The obtained glass powder was heated to 1200 ℃ at a rate of 10 ℃ / min using DSC to obtain the glass transition temperature (T1=1017 K) and the crystallization initiation temperature (T2=1033 K). (4) The melting temperature (T3=1716 K) was measured using a melting point apparatus, and the spinnability parameter (H=0.093) was calculated. It was predicted that this coal gasification slag could not be spun into basalt fiber, but this coal gasification slag was spinnable, so the prediction failed.

[0026] By comparing Comparative Example 1 and Example 2, the applicant's claim regarding the influence of crystals in the raw materials can be verified. The initial crystals inside the raw materials that have not undergone melting treatment will cause a significant decrease in T2, resulting in a deviation in the calculation of the H value.

[0027] The comparison between Comparative Example 2 and Example 2 further confirms the applicant's idea about the influence of crystals in the raw materials. Insufficient melting time means that there are still incompletely melted microcrystals in the raw materials. These microcrystals also promote the formation of crystals, resulting in a significant decrease in T2, which leads to a deviation in the calculation of H value and thus the prediction fails.

[0028] Although embodiments of the present invention have been shown and described above, it is understood that the above embodiments are exemplary and should not be construed as limiting the present invention. Those skilled in the art can make changes, modifications, substitutions and variations to the above embodiments within the scope of the present invention.

Claims

1. A quantitative analysis method for the spinnability of continuous basalt fiber raw materials, characterized in that, Includes the following steps: S1: Basalt fiber raw material is heated and melted, and then quenched in water to obtain a glassy substance; S2: The glass body is crushed to obtain glass powder; S3: The glass powder is heated, and during the heating process, thermal signals are collected using thermal analysis methods to obtain the glass transition temperature T1 and the crystallization initiation temperature T2. S4: Calculate the spinnability parameter H by combining the glass transition temperature T1, the initial crystallization temperature T2, and the complete melting temperature T3 of the raw material, and evaluate it.

2. The method according to claim 1, characterized in that, In step S1, the basalt fiber raw material includes one or more combinations of single basalt ore, artificial compounding materials, or solid waste.

3. The method according to claim 2, characterized in that, In step S1, the combination includes one or two combinations of basalt ore and artificial batching materials or solid waste.

4. The method according to claim 2 or 3, characterized in that, In step S1, the solid waste includes coal gasification ash.

5. The method according to claim 1, characterized in that, In step S1, the heating and melting process involves heating to 1500-1650℃ and holding at that temperature for 6-16 hours.

6. The method according to claim 1, characterized in that, In step S2, the particle size of the glass powder is 200-250 mesh.

7. The method according to claim 1, characterized in that, In step S3, the heating is heating to above 1200°C; And / or, the heating rate is 5-20 °C / min.

8. The method according to claim 1, characterized in that, In step S3, the thermal analysis method includes differential scanning calorimetry or differential thermal analysis.

9. The method according to claim 1, characterized in that, In step S4, the method for calculating the spinnability parameter H is as follows: H=(T2-T1) / T3, If H > 0.01, the raw material is spinnable; if H ≤ 0.01, the raw material is not spinnable.

10. The method according to claim 1, characterized in that, In step S4, the complete melting temperature T3 is measured by a melting point apparatus or obtained by thermodynamic calculation.

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