Method for improving production efficiency and fiber performance of continuous basalt fiber through multi-element mixing of raw materials

By diversifying magmatic rock raw materials with different SiO2 contents, the spinability defects and component volatility problems of single basalt fiber ore raw materials are solved, and the production efficiency and fiber performance of continuous basalt fibers are improved.

CN119638180AActive Publication Date: 2025-03-18四川省能源地质调查研究所
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Patent Information

Application Number
CN202411805848.1
Authority / Receiving Office
CN · China
Patent Type
Applications(China)
Current Assignee / Owner
Filing Date
2024-12-10
Publication Date
2025-03-18
Estimated Expiration
2044-12-10

AI Technical Summary

Technical Problem

The spinning defects of single basalt fiber ore raw materials and the volatility of mineral and chemical composition lead to low production efficiency and unstable fiber performance of continuous basalt fibers.

Method used

By selecting the basic-neutral magmatic rocks with different mass percentages of SiO2 as the main material and batching, performing multi-combination, adjusting the chemical composition content, improving the homogeneity and thermal conductivity of the glass liquid, thereby improving the production efficiency and fiber performance of continuous basalt fibers.

Benefits of technology

Through multi-combination, the fiber wire formation and full barrel rate are improved, the fiber performance is stabilized, and the glass liquid homogeneity and thermal conductivity are significantly improved during the wire drawing production process.

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Abstract

The invention belongs to the field of inorganic non-metallic materials, and particularly relates to a method for improving the production efficiency and the fiber performance of continuous basalt fibers through multi-element mixing of raw materials. Through multi-component mixing of different raw materials, the percentage content of main oxides of raw material minerals, namely the percentage content of network former, network intermediate and network modifier oxides, and the ratio of main ore raw materials FeO / (Fe2O3 + FeO) are properly adjusted; the spinnability defects that in a single mineral raw material, the ratio of 2 + valent iron to 3 + valent iron is unbalanced, the content of main oxides such as SiO2 and Al2O3 is slightly low, and the content of alkaline earth oxides such as CaO and MgO is unbalanced are overcome, so that the homogeneity and the thermal conductivity of molten glass in the wire drawing production process are greatly improved, the wire drawing operation stability of the basalt fiber is improved, and the quality of the basalt fiber is improved. Therefore, the filament forming rate and the full barrel rate of the fibers are improved, and the performance of the basalt fibers is synchronously stabilized.
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Description

Technical Field

[0001] The invention belongs to the field of inorganic non-metallic materials, and specifically relates to a method for improving the production efficiency and fiber performance of continuous basalt fibers by multi-component mixing of raw materials. Background Art

[0002] As an inorganic high-performance fiber with excellent physical and chemical properties, basalt fiber has shown broad application prospects in many fields such as national defense and military industry, transportation, fire protection and heat insulation, electricity and new energy, national infrastructure construction, marine and maritime affairs, dielectric materials, and automobile manufacturing, demonstrating huge industrial development potential.

[0003] A large number of production practices have proved that the ore raw materials of continuous basalt fiber are not limited to basalt. Many magmatic rocks including diabase, gabbro, basaltic andesite, andesite, gray-green diorite, pyroxene diorite, diorite, etc. can be used for continuous basalt fiber production. In terms of raw materials, the existing basalt fiber preparation methods in my country all use a single ore raw material for continuous basalt fiber production. However, due to its natural nature, single basalt ore has spinnability defects. At the same time, natural ores will inevitably have fluctuations in mineral and chemical composition. The spinnability defects and composition fluctuations of raw materials seriously affect the production efficiency and fiber performance of continuous basalt fiber. Under the premise of continuing the "naturalness" and green environmental protection of basalt fiber, in order to obtain higher production efficiency and stabilize fiber quality, it is necessary to design the ideal raw material mineral and chemical composition content to improve the difficulty of continuous basalt fiber drawing and poor drawing effect, so as to improve the production efficiency and fiber performance of continuous basalt fiber. Summary of the invention

[0004] In order to overcome the spinnability defects of single basalt fiber ore raw materials and the impact of fluctuations in mineral and chemical composition on production, the present invention improves the stability of continuous basalt fiber drawing operations through multi-mixing of raw materials, thereby improving the fiber yarn formation rate and full barrel rate, and simultaneously stabilizing the basalt fiber performance.

[0005] Specifically, the technical solution adopted by the present invention is: a method for improving the production efficiency and fiber performance of continuous basalt fiber by multi-mixing of raw materials, the method comprising the following steps:

[0006] (1) Raw material selection: one or more basic-neutral igneous rocks with a SiO2 content of greater than or equal to 52% and less than 54% by mass are selected as the main material, one or more neutral igneous rocks with a SiO2 content of greater than or equal to 54% and less than 58% by mass are selected as the first ingredient, and optionally, one or more basic igneous rocks with a SiO2 content of greater than or equal to 47% and less than 52% by mass are selected as the second ingredient;

[0007] (2) Raw material ratio: Determine the chemical composition content of the main ingredient and the ingredients selected in step (1) by material testing means, and determine the ratio of the main ingredient and the ingredients based on the target component content of the mixed ingredients;

[0008] (3) Mixing: Mix the raw materials in the right proportions, crush and grind them, and homogenize the resulting powder;

[0009] (4) Fiber production: The mixed powder obtained in step (3) is subjected to wire drawing to obtain continuous basalt fibers.

[0010] As used herein, basic igneous rock, basic-neutral igneous rock, and neutral igneous rock refer to conventional rock classifications of igneous rocks in the art based on the mass percentage content of silicon dioxide.

[0011] Furthermore, the basic-intermediate igneous rock includes basalt, basaltic andesite, gray-green andesite or pyroxene andesite.

[0012] Furthermore, the neutral rock includes andesite or diorite.

[0013] Furthermore, the basic rock includes basalt, diabase or gabbro.

[0014] Further, the mass fraction of total iron in the main material is 8%-11%, and the mass fraction of total iron in the ingredients (e.g., the first ingredient or the second ingredient) is 6%-13%. As used herein, total iron refers to the total mass fraction of Fe2O3 and FeO in the ore.

[0015] Furthermore, the mineral structure of the main material is dense or obliquely porphyritic, and the mineral structure of the ingredient (for example, the first ingredient or the second ingredient) is dense or obliquely porphyritic.

[0016] Furthermore, the ignition loss of the main ingredient and the supplementary ingredients is ≤2.0%.

[0017] Furthermore, the target content of each chemical component in the mixed material of the main ingredient and the ingredients in step (2) is: by mass percentage, 52%-55% SiO2, 15%-17% Al2O3, 7%-10.5% Fe2O3+FeO, 11%-16% MgO+CaO, 3%-6% K2O+Na2O, and 1%-4% TiO2.

[0018] Furthermore, the target component content of the mixed material is, by mass, FeO / (Fe2O3+FeO)=0.4-0.8.

[0019] Furthermore, in the target component content of the mixed material, the mass fraction of plagioclase + pyroxene is ≥ 70%.

[0020] Furthermore, in step (3), the powder has a particle size of 80-100 mesh.

[0021] As used herein, the mixed powder is subjected to wire drawing production using conventional processes well known in the art, for example, the wire drawing production can be carried out using melting, wire drawing forming, and infiltration coating process means.

[0022] In other aspects, the present invention also provides continuous basalt fibers produced by the methods described herein.

[0023] Advantageous Effects of the Invention

[0024] The present invention mixes different raw materials, appropriately adjusts the mass percentage content of the main oxides of the raw material minerals, i.e., the mass percentage content of the oxides of the network formers, network intermediates and network modifiers, and the ratio of the main ore raw material FeO / (Fe2O3+FeO), thereby correcting the spinnability defects of the single mineral raw material, such as the imbalance of the ratio of 2+ valent iron to 3+ valent iron, the slightly low content of the main oxides such as SiO2 and Al2O3, and the imbalance of the content of alkaline earth oxides such as CaO and MgO, thereby greatly improving the homogeneity and thermal conductivity of the glass liquid in the wire drawing production process, thereby improving the production efficiency and fiber performance of the continuous basalt fiber. DETAILED DESCRIPTION

[0025] The present invention is further described below with reference to specific examples, but the examples do not limit the present invention in any form. Unless otherwise specified, the reagents, methods and equipment used in the present invention are conventional reagents, methods and equipment in the art.

[0026] Example:

[0027] The present invention provides a method for improving the production efficiency and fiber performance of continuous basalt fiber by multi-component mixing of raw materials, comprising:

[0028] (1) Raw material selection: In this embodiment, the basalt ore from Weixian County, Hebei Province used in the production of Sichuan Juyuan Basalt Fiber Technology Co., Ltd. is selected as the main material, and ores from several representative basalt mines in Sichuan Province are selected as the ingredients. Specific information is shown in Table 1.

[0029] Table 1: Mineral Points for Mixed Raw Materials

[0030] Serial number Ore Land Rock Type Remark 1# Suluo basalt mine in Meigu County, Sichuan Province Basalt Ingredients 2 2# Hebei Weixian Basalt Mine Basalt Ingredients 3# Xiangzhangping basalt mine in Hanyuan County, Sichuan Province Basaltic andesite Ingredients 1-1 4# Zengheba diorite in Jinkouhe District, Sichuan Province Diorite Ingredients 1-2

[0031] (2) Determine the content of each component in each ore. See Table 2.

[0032] Table 2: Content of each component in the mixed ore

[0033]

[0034] (3) Ingredients: According to the target content (i.e., ≥70% plagioclase + pyroxene; 52%-55% SiO2, 15%-17% Al2O3, 7%-10.5% Fe2O3+FeO, 11%-16% MgO+CaO, 3%-6% K2O+Na2O, 1%-4% TiO2, FeO / (Fe2O3+FeO)=0.4-0.8), the mass percentage of each mixed ingredient is calculated according to the content of each component in Table 2. As shown in Table 3, according to mass percentage, Example 1 weighs 28 parts of 1# ingredient, 32 parts of 2# main ingredient, and 40 parts of 3# ingredient for mixing; Example 2 weighs 12 parts of 1# ingredient, 21 parts of 2# main ingredient, 28 parts of 3# ingredient, and 39 parts of 4# ingredient for mixing. The comparative example is composed of only the main ingredient.

[0035] Table 3: Weight percentage of the ore

[0036] Ore Point Example 1 Example 2 Comparative Example 1#(matching) 28 12 0 2#(main) 32 21 100 3#(matching) 40 28 0 4#(matching) 0 39 0

[0037] (4) The mixed materials of Example 1 and Example 2 were ground and mixed evenly, and then sampled and tested after sieving (80-100 mesh) to ensure that the content of each component of the mixed materials was within the required range (if the requirements were not met, secondary mixing was required), and mixed powder was obtained. The test results of the content of each component in each embodiment are shown in Table 4.

[0038] Table 4: Test results of the content of each component of the mixed powder in each embodiment

[0039] Component (%) Example 1 Example 2 Comparative Example <![CDATA[SiO2]]> 52.32 54.05 52.52 <![CDATA[Al2O3]]> 16.31 16.30 16.35 <![CDATA[Fe2O3]]> 4.25 3.87 3.01 FeO 5.13 4.51 6.44 <![CDATA[K2O]]> 0.87 0.84 0.68 <![CDATA[Na2O]]> 2.58 2.57 2.48 CaO 9.05 7.77 8.55 MgO 6.80 7.08 6.88 <![CDATA[TiO2]]> 1.83 1.81 2.22 LOI 0.85 1.20 0.89

[0040] (5) Wire drawing production: The mixed powder obtained in the previous step is gradually added to the pool kiln. After the raw materials in the pool kiln are completely replaced, the wire drawing production is carried out by means of melting, wire drawing forming, and impregnation coating processes. The production parameters are recorded to obtain continuous basalt fibers.

[0041] (6) The production efficiency and fiber properties of basalt fiber were tested, and the results are shown in Table 5.

[0042] Table 5: Basalt fiber production efficiency and fiber properties of each example

[0043] Example 1 Example 2 Comparative Example Melt T 1436℃ 1468℃ 1458℃ Molding T 1208℃ 1278℃ 1267℃ Liquidus T 1118℃ 1162℃ 1178℃ Fiber φ 13μm 13μm 13μm Fiber forming rate 94% 92% 83% Full barrel rate 94.4% 88.8% 27.8% Tensile Strength 2580MPa 2820MPa 2464MPa Tensile modulus 84GPa 90GPa 81GPa

[0044] As can be seen from Table 5, in Example 1, by mixing, the mass percentage content of the single main ore raw material network former, network intermediate and network altered oxide is appropriately adjusted, and the ratio of the main ore raw material FeO / (Fe2O3+FeO) is greatly reduced, that is, the ratio of the main ore raw material FeO / (Fe2O3+FeO) in the comparative example 2 is corrected. + Valence iron and 3+ The two spinnability defects of unbalanced iron ratio and CaO imbalance are eliminated, so that the homogeneity and thermal conductivity of the glass liquid in the drawing process are greatly improved, which is manifested in the reduction of gas and electricity consumption in the production process, the improvement of fiber forming rate, especially the fiber full barrel rate has been geometrically increased, and the performance of some fibers (tensile strength and tensile modulus) has also been improved to a certain extent. The drawing effect is significantly better than the comparative example.

[0045] In Example 2, by mixing, the mass percentage content of the framework oxide SiO2 in the comparative example is moderately increased, and the ratio of FeO / (Fe2O3+FeO) is significantly reduced, and the ratio of FeO / (Fe2O3+FeO) in the comparative example 2 is corrected. + Valence iron and 3 + The two spinnability defects of unbalanced valence iron ratio and unbalanced framework oxides are eliminated, so that the homogeneity and thermal conductivity of the glass liquid in the production process are improved, which is manifested in the obvious enhancement of fiber tensile strength, the improvement of filament formation rate, the geometric growth of fiber full barrel rate, and the significant improvement of some fiber properties (tensile strength and tensile modulus properties). The wire drawing effect is significantly better than that of the comparative example.

[0046] It should be noted that the preferred embodiments of the present invention are given in the specification of the present invention, but the present invention can be implemented in many different forms and is not limited to the embodiments described in this specification. These embodiments are not intended to be additional limitations on the content of the present invention. The purpose of providing these embodiments is to make the understanding of the disclosure of the present invention more thorough and comprehensive. In addition, the above-mentioned technical features continue to be combined with each other to form various embodiments not listed above, which are all considered to be within the scope of the present invention specification; further, for ordinary technicians in this field, they can be improved or transformed according to the above description, and all these improvements and transformations should belong to the protection scope of the claims attached to the present invention.

Claims

1. A method for improving the production efficiency and fiber performance of continuous basalt fiber by multi-component mixing of raw materials, characterized in that: The method comprises the following steps: (1) Raw material selection: one or more basic-neutral igneous rocks with a SiO2 content of greater than or equal to 52% and less than 54% by mass are selected as the main material, one or more neutral igneous rocks with a SiO2 content of greater than or equal to 54% and less than 58% by mass are selected as the first ingredient, and optionally, one or more basic igneous rocks with a SiO2 content of greater than or equal to 47% and less than 52% by mass are selected as the second ingredient; (2) Raw material ratio: Determine the chemical composition content of the main ingredient and the ingredients selected in step (1) by material testing means, and determine the ratio of the main ingredient and the ingredients based on the target component content of the mixed ingredients; (3) Mixing: Mix the raw materials in the right proportions, crush and grind them, and homogenize the resulting powder; (4) Fiber production: The mixed powder obtained in step (3) is subjected to wire drawing to obtain continuous basalt fibers.

2. The method according to claim 1, characterized in that The basic-intermediate igneous rock includes basalt, basaltic andesite, gray-green andesite or pyroxene andesite; The neutral igneous rock includes andesite or diorite; The basic igneous rock includes basalt, diabase or gabbro.

3. The method according to claim 1, characterized in that: The mass fraction of total iron in the main material is 8%-11%, and the mass fraction of total iron in the auxiliary material is 6%-13%.

4. The method according to claim 1, characterized in that The mineral structures of the main material and the supplementary materials are dense or porphyritic.

5. The method according to claim 1, characterized in that: The ignition loss of the main ingredient and the supplementary ingredients is ≤2.0%.

6. The method according to claim 1, characterized in that The target component contents of the mixed materials in step (2) are: by mass percentage, 52%-55% SiO2, 15%-17% Al2O3, 7%-10.5% Fe2O3+FeO, 11%-16% MgO+CaO, 3%-6% K2O+Na2O, and 1%-4% TiO2.

7. The method according to claim 6, characterized in that The target component content of the mixed material is, by mass, FeO / (Fe2O3+FeO)=0.4-0.8; Furthermore, in the target component content of the mixed material, the mass fraction of plagioclase + pyroxene is ≥ 70%.

8. The method according to claim 1, characterized in that In step (2), the main ingredient, the first ingredient and optionally the second ingredient are mixed in a ratio of 20%-80%: 10%-50%: 0%-30%.

9. The method according to claim 1, characterized in that: In step (3), the powder has a particle size of 80-100 mesh.

10. A continuous basalt fiber produced by the method of any one of claims 1-9.

Citation Information

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