CN115032362A - Uniformity control method of ore raw material for basalt fiber - Google Patents

Uniformity control method of ore raw material for basalt fiber Download PDF

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CN115032362A
CN115032362A CN202210362374.2A CN202210362374A CN115032362A CN 115032362 A CN115032362 A CN 115032362A CN 202210362374 A CN202210362374 A CN 202210362374A CN 115032362 A CN115032362 A CN 115032362A
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孟亚平
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Abstract

The invention discloses a method for controlling the uniformity of an ore raw material for basalt fibers, which comprises the following steps: step 1: selecting a plurality of preset ore raw materials, and mixing and homogenizing the selected ore raw materials according to a preset proportion to prepare a primary mixed raw material; step 2: taking five samples in the primary mixed raw materials, crushing each sample, and processing into micro powder to form a secondary mixed raw material; and step 3: taking five subsamples in the secondary mixed raw material, respectively calculating chemical component tests of oxides in the subsamples, and judging whether homogenization is completed according to chemical component test results; and if the chemical composition test result does not meet the requirement, repeating the step 1 to the step 3. According to the method, a microcosmic component control process is not needed, various ores are matched according to a proper proportion in a macroscopic view, whether homogenization is completed or not is judged according to the oxide content of the subsamples in the sample after homogenization, and if homogenization is not completed, the homogenization process is repeated, so that the method has high practicability.

Description

Uniformity control method of ore raw material for basalt fiber
Technical Field
The invention relates to the technical field of basalt fiber production, in particular to a component uniformity control method of an ore raw material for manufacturing continuous basalt fiber by an electric melting tank furnace method.
Background
The basalt fiber is continuous fiber drawn from one or more natural basalt ores, and is formed by melting the basalt ores at 1450-1500 ℃ and drawing the basalt ores at high speed through a platinum-rhodium alloy wire drawing bushing. The basalt fiber is a novel inorganic environment-friendly green high-performance fiber material and is composed of oxides such as silicon dioxide, aluminum oxide, calcium oxide, magnesium oxide, ferric oxide, titanium dioxide and the like. The basalt continuous fiber has high mechanical property, and also has various excellent properties of electrical insulation, corrosion resistance, high temperature resistance and the like. In addition, the production process of the basalt fiber determines zero emission, no solid waste and environmental friendliness, and the product can be directly degraded in the environment after being discarded without any harm, so that the basalt fiber is a real green and environment-friendly material. Basalt fibers are taken as one of four major (carbon fibers, aramid fibers, ultra-high molecular weight polyethylene and basalt fibers) high-technology and high-performance fibers which are mainly developed in China, and industrial production is realized. The basalt continuous fiber has been widely applied in various aspects such as fiber reinforced composite materials, road engineering, construction fields, friction materials, shipbuilding materials, heat insulation materials, automobile industry, high-temperature filter fabrics, protection fields and the like, and is an industrial material in the twenty-first century.
Among basalt fiber components, Al 2 O 3 、SiO 2 The content of FeO (Fe) reaches 70 percent 2 O 3 ) The content is more than 10 percent, R 2 O (alkali metal oxide) is only 5 to 6% or less. The basalt fiber has poor heat-conducting property, short material property, strong crystallization tendency, high crystallization upper limit temperature, poor electric conductivity and other poor processing properties, so the production level of the basalt fiber is far lower than that of the E glass fiber at present.
In view of the above, the existing production process of basalt fibers mostly adopts a small-scale production process, a furnace heating mode or flame heating or electric heating adopts a process of shallow liquid level, single-layer wall body, non-propulsive rod-shaped or plate-shaped electrode and horizontal melting, a wire drawing bushing mainly comprises 400 holes and 200 holes, the daily yield of a single furnace is only 0.3-0.4 ton, and the problems which need to be solved urgently are caused by serious pollution (flame heating), high cost, low yield, short furnace life, unstable performance, poor quality and the like, and the production process is far lower than the requirement of the market on large-scale production.
Therefore, the inventor of the invention, which is previously applied for patent application No. CN202110068680.0, discloses an electric melting furnace for producing continuous basalt fibers, which comprises a furnace body and an electric melting control device, wherein a melting tank, a material channel, a working material channel and a working chamber are sequentially arranged in the furnace body, a feeding part is arranged above the melting tank, and a blocking brick is arranged between the melting tank and the material channel; the blocking brick is provided with a central part for accommodating the cooling device and a peripheral structure for wrapping the central part; the top of the blocking brick is fixed on the inner wall of the top of the melting tank, and the bottom of the blocking brick and the bottom of the melting tank are provided with preset heights for conducting the solution. Through the structure, the structure of the throat and the electrode in the prior art is improved, and the distance from the bottom of the melting tank to the material channel is 4/5 shorter than that of the throat structure due to the addition of the baffle structure. The electrode arrangement of unilateral makes the heating more even, and both improvements have all reduced thermal loss, consequently, not only greatly reduced the construction cost of electric melting kiln stove, still reduced the loss of energy consumption, improved the production efficiency of producing continuous fibers. The production of the basalt fiber with low cost and high efficiency can be realized. The invention adopts a kiln adopting an electric melting process and a wire drawing technology, and provides a new way for a large-scale basalt fiber production technology.
The basalt fiber and the glass fiber have the characteristics of similar properties and most of the application fields are overlapped. The development of basalt fiber needs to realize production scale, so that the cost is changed into glass fiber, and the glass fiber has market competitiveness with glass fiber. Tank kilning of the manufacturing process must be achieved to achieve this goal. The objectives of tank furnace melting must include process stability, long life of the furnace, long life of the bushing, ease of melting of the ore raw materials, stable product performance, excellent product quality, and the like. Therefore, in the actual production process, the homogenization of the components of the ore raw material is required to be realized so as to realize the optimization of the melting process, the optimization of the fusant, the optimization of the product performance and the optimization of the product quality. Generally, materials are various ores, so that an important problem in practical application is to homogenize various ores macroscopically and ensure that the raw material ratio of the homogenized ores meets the operation requirement of a kiln so as to realize the stability and continuity of the wire drawing operation in a wire drawing operation window.
The kiln production process in the prior art usually microscopically requires and standardizes the components of ore raw materials, however, the existing ore raw materials for producing basalt fibers all adopt natural raw materials, have large component fluctuation, cannot completely meet the requirements of the production process, and cannot meet the requirements of the tank kiln process of large-scale industrial production. The components of natural ore are not standard, and the large fluctuation of the components is always a fundamental technical bottleneck for the large-scale development of the basalt fiber industry. Therefore, the prior art control process aiming at the components on the micro scale is difficult to control and realize in the actual production.
Disclosure of Invention
The following presents a simplified summary of embodiments of the invention in order to provide a basic understanding of some aspects of the invention. It should be understood that the following summary is not an exhaustive overview of the invention. It is not intended to determine the key or critical elements of the present invention, nor is it intended to limit the scope of the present invention. Its sole purpose is to present some concepts in a simplified form as a prelude to the more detailed description that is discussed later.
The prior art aims at the problem that the microcosmic component control process is difficult to control and realize in actual production, so that the ore raw material components for manufacturing the continuous basalt fibers by the electric melting furnace technology are designed, the basalt ore is adopted for homogenization, the optimization determination of the ore raw material components and the homogenization of the ore components can be realized by the homogenization method macroscopically, and the embarrassment of the actual production of the basalt fibers is expected to be changed.
In order to solve the technical problem, the present application provides a method for controlling uniformity of an ore raw material for basalt fiber, the method comprising:
step 1: selecting a plurality of preset ore raw materials (two or more than two ore raw materials), and mixing and homogenizing the selected ore raw materials according to a preset proportion to prepare a primary mixed raw material; the granularity of the primary mixed raw material is 1-3 mm; the mixing method of mixing and homogenizing the raw materials to be preliminarily mixed can be realized by adopting a conventional mechanical stirring method or a material flow mixing method or a pneumatic mixing method (an air flow method);
step 2: taking five samples in the primary mixed raw materials, crushing each sample, and processing the samples into micro powder to form a secondary mixed raw material; wherein each sample is selected in kilogram order;
and 3, step 3: taking five subsamples of the secondary mixed raw material, and respectively calculating the chemical composition test of each oxide in the subsamples, wherein the oxide is SiO 2 、CaO、MgO、Al 2 0 3 、Fe 2 O 3 、FeO、Na 2 O、K 2 O or TiO 2 Judging whether homogenization is finished or not according to a chemical component test result; if the chemical composition test result does not meet the requirement, repeating the step 2 and the step 3; if the chemical composition test results meet the requirements, the homogenization is completed.
Specifically, step 3 includes calculating:
Figure RE-GDA0003734818200000041
wherein A is in An oxide representing the ith (1. ltoreq. i.ltoreq.5) child sample of the nth (1. ltoreq. n.ltoreq.5) sample, the oxide being SiO 2 、CaO、MgO、Al 2 0 3 、Fe 2 O 3 、FeO、Na 2 O、K 2 O or TiO 2
Figure DA00035844000156072786
Represents the average value of a certain oxide in the n (1. ltoreq. n.ltoreq.5) th sample, K in Representing the dispersion coefficient of the ith (1. ltoreq. i.ltoreq.5) subsample in the nth (1. ltoreq. n.ltoreq.5) sample; and the dispersion coefficient K of each oxide in the ith (1. ltoreq. i.ltoreq.5) subsample in the nth (1. ltoreq. n.ltoreq.5) sample in Satisfies the following conditions:
SiO 2 Al 2 0 3 CaO MgO (Fe 2 O 3 +FeO) Na 2 O K 2 O TiO 2
K in 0.5% 1% 2% 2% 2.5% 3% 3% 3%
further, step 3 further comprises: calculating out
Figure RE-GDA0003734818200000051
B represents the average of certain oxides of five samples, f n Denotes the n (1. ltoreqn is less than or equal to 5) dispersion coefficients of the average value of certain oxides in the samples; and the dispersion coefficient f of the average value of each oxide in the n (1. ltoreq. n. ltoreq.5) th sample n Satisfies the following conditions:
SiO 2 Al 2 0 3 CaO MgO (Fe 2 O 3 +FeO) Na 2 O K 2 O TiO 2
f n 1% 2% 4% 4% 5% 6% 6% 6%
in practical implementation, the preset multiple ore raw materials are selected to be 140-210 tons in batch (the batch is calculated by 20-30 times according to the model of a kiln and the daily output), and each obtained sample is fully stirred and homogenized in a small mechanical stirring or ball milling stirrer. After the homogenization process is finished, five samples are randomly sampled, each sample is 5-10 Kg, and the samples are crushed and ground until the granularity is less than or equal to 200 meshes. Taking five sub-samples at random from the fully homogenized five samples, performing chemical composition test on the sub-samples, and determining the SiO of the sub-samples 2 、Al 2 O 3 、CaO、MgO、Fe 2 O 3 、FeO、TiO 2 、 K 2 O、Na 2 O、MnO 2 The content of (b). By adopting the scheme and matching with the electric melting tank furnace, stable and efficient continuous basalt fiber production can be realized. Actual tests show that the dispersion of the original filament strength is less than or equal to 3%, the dispersion of the elastic modulus is less than or equal to 3%, the wiredrawing yield is greater than or equal to 92%, wiredrawing operation with the specification of 7-22 μm is realized, the drawplate is suitable for the bushing operation with 400-2400 holes, the drawplate operation with 400-2400 holes is suitable, the wiredrawing yield is greater than or equal to 92%, the service life of a kiln is 3-4 years, the service life of the bushing is 6-8 months, the original filament strength is 2200-3300 MPa, the elastic modulus is 86-96 Pa, and ten thousand tons of basalt fibers can be produced annually.
Further, the average value of an oxide in five samples was further calculated as follows:
Figure RE-GDA0003734818200000052
wherein A is in An oxide of the ith (1. ltoreq. i.ltoreq.5) child sample of the nth (1. ltoreq. n.ltoreq.5) sample,
Figure RE-GDA0003734818200000053
represents the average value of a certain oxide in the n-th (1. ltoreq. n.ltoreq.5) sample.
When in use, the batch of the materials is 1/3 with daily output within 5 tons every time, multiple materials are adopted, and the conventional mechanical stirring or pneumatic (air flow) homogenization method can be adopted. When the raw material batches are replaced, the proportion and the weight of the batch materials are recalculated according to the patent requirements. The water content is measured during calculation, and the weight of the dried raw materials is taken as the basis for calculation.
In the method, the particle size (the particle size refers to the size of particles, the particle size of spherical particles is generally represented by diameter, the particle size of cubic particles is represented by side length, and the diameter of a certain sphere having the same behavior as the particles can be used as the equivalent diameter of the particles for irregular particles) of the basalt ore is controlled to be 0.5-3 mm. The granularity is controlled to be 0.5-3 mm, so that raw materials are melted, dust is controlled, and automatic feeding is facilitated.
The method for controlling the uniformity of the components of the ore raw material for manufacturing the continuous basalt fiber by the tank furnace method is characterized in that five fully homogenized samples are randomly taken, chemical component test is carried out on the samples, and the SiO of the samples is measured 2 、Al 2 O 3 、CaO、MgO、Fe 2 O 3 、FeO、TiO 2 、K 2 O、Na 2 O、 MnO 2 The content of (b). The homogeneity and content of 5 corresponding oxide reaction subsamples in the subsample were determined. In the method, the test results of five subsamples are obtained according to calculation
Figure RE-GDA0003734818200000061
And K in Thereby reflecting the uniformity of the subsamples while the uniformity accuracy requirement (K) for each oxide of the five subsamples is determined in ) The sample uniformity meets the requirements, and the homogenization result of the subsample can meet the requirements of process judgment. The dispersion coefficient f of the average value of certain oxide in the nth sample obtained by calculation n And an average oxide content B.
Through the scheme, the batch homogenization reaches the homogenization of 5-10 kg (five samples) in macroscopic scale, the precise and sufficient homogenization reaches the homogenization of 5-10 g (five samples) in macroscopic scale, and the content of corresponding oxides is expressed. Micro-homogenization, i.e. homogenization at the molecular level, in the electric melting tank furnace through the designed heat convection area and furnace of the electric melting tank furnaceAnd the convection and diffusion of the whole liquid flow process are realized. f. of n The uniformity of 5-10 kg in macroscopic scale is expressed. K in Expresses the precise and sufficient homogenization of 5-10 g (pentagram) in macroscopic scale. B expresses the oxide content of the whole kiln.
The scheme of the application is particularly used for solving the problems that the existing natural ore raw material for producing basalt fibers has large component fluctuation, the components can not completely meet the requirements of the production process, and the requirements of a tank furnace process of large-scale industrial production can not be met 2 O 3 、SiO 2 And the micro proportioning data of mineral components is obtained, a micro component control process is not needed, a plurality of ores are only needed to be matched according to a proper proportion in a macroscopic view, whether homogenization is completed or not is judged according to the oxide content of a subsample in a sample after homogenization, and if homogenization is not completed, the homogenization process is repeated, so that the method has very good practicability.
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The invention may be better understood by referring to the following description in conjunction with the accompanying drawings, in which like reference numerals are used throughout the figures to indicate like or similar parts. The accompanying drawings, which are incorporated in and form a part of this specification, illustrate preferred embodiments of the present invention and, together with the detailed description, serve to further explain the principles and advantages of the invention. On the attachment
In the figure:
FIG. 1 is a top view of an electric melting furnace of the present invention;
FIG. 2 is a perspective view of an electric melting furnace of the present invention.
Detailed Description
Embodiments of the present invention will be described below with reference to the accompanying drawings. Elements and features depicted in one drawing or one embodiment of the invention may be combined with elements and features shown in one or more other drawings or embodiments. It should be noted that the figures and description omit representation and description of components and processes that are not relevant to the present invention, but known to those of ordinary skill in the art, for the sake of clarity.
In the description of the present invention, it should be noted that, unless otherwise explicitly specified or limited, the terms "mounted," "connected," and "connected" are to be construed broadly, e.g., as meaning either a fixed connection, a removable connection, or an integral connection; can be mechanically or electrically connected; they may be connected directly or indirectly through intervening media, or they may be interconnected between two elements. The specific meanings of the above terms in the present invention can be understood in specific cases to those skilled in the art.
Referring to fig. 1, an embodiment of the present invention provides a method for controlling uniformity of an ore raw material for basalt fiber, including:
step 1: selecting a plurality of preset ore raw materials (two or more than two ore raw materials), and mixing and homogenizing the selected ore raw materials according to a preset proportion to prepare a primary mixed raw material; the particle size of the primary mixed raw material is 1-3 mm; the mixing method of mixing and homogenizing the raw materials to be preliminarily mixed can be realized by adopting a conventional mechanical stirring method or a material flow mixing method or a pneumatic mixing method (an air flow method);
step 2: taking five samples in the primary mixed raw materials, crushing each sample, and processing into micro powder to form a secondary mixed raw material; wherein each sample is selected in kilogram order;
and 3, step 3: taking five sub-samples in the secondary mixed raw material, and respectively calculating the chemical composition test of each oxide in the sub-samples, wherein the oxide is SiO 2 、CaO、MgO、Al 2 0 3 、Fe 2 O 3 、FeO、Na 2 O、K 2 O or TiO 2 Judging whether homogenization is finished or not according to a chemical component test result; if the chemical component test result does not meet the requirement, repeating the step 1 to the step 3; if the chemical composition test results meet the requirements, the homogenization is completed.
The preliminary mixed raw material in step 1 may be a preliminary mixed raw material obtained by pretreating a plurality of ore raw materials, and the embodiment employs a stratified stacking which is divided into three or more grades (for example, a grade) according to the content of an oxide component:SiO 2 The content is more than the preset value 1, and the grade B is as follows: SiO 2 2 The content is less than the preset value 1 and greater than the preset value 2, and the grade C is as follows: SiO 2 2 The content is less than the preset value 2), and then the raw materials of the three grades are respectively piled up in a layered way: the raw material of the A grade is placed at the top, the raw material of the B grade is placed in the middle, and the raw material of the C grade is placed at the bottom; the mixed raw material obtained by the pretreatment scheme can be matched with subsequent processing to a greater extent.
The method is applied to an electric melting furnace, and the electric melting furnace comprises a furnace body 100 and an electric melting control device 200, wherein a melting tank 101, a material channel 102, a main material channel 103 and a working chamber 104 are sequentially arranged in the furnace body 100, a feeding part is arranged above the melting tank 101, a feeding port 105 is arranged at the top of the furnace body 100, and the feeding part comprises a feeding device for feeding materials into the feeding port 105, and the feeding device is shown in fig. 1. A blocking brick 300 is arranged between the melting tank 101 and the material channel 102. The working chamber 104 has a plurality of forming areas, each forming area is provided with a bushing 107, the forming areas are separately separated, and the working chamber 104 is at least provided with more than 2 forming areas.
The homogenization batch of the ore raw materials is 20-30 times of the daily production of the tank furnace, and the granularity requirement of the ore raw materials is as follows: 0.5-3 mm. The homogenization adopts a conventional mechanical stirring method or a logistics mixing method or a pneumatic mixing method (an airflow method), five samples are taken after the homogenization, each sample is 5-10 Kg, each sample is crushed and processed into micro powder, five sub-samples are taken from each sample, and the calculation is respectively carried out:
Figure RE-GDA0003734818200000091
Figure RE-GDA0003734818200000092
where A is in Represents a certain oxide of the ith sub-sample in the nth sample, for example: SiO 2 2 CaO, MgO, etc.,
Figure RE-GDA0003734818200000093
represents the nth sampleAverage value of certain oxide in the product, B represents average value of certain oxide in five samples, K in Representing the coefficient of dispersion, f, of the ith subsample in the nth sample n A coefficient of dispersion representing an average value of a certain oxide in the nth sample, K of each oxide in And f n Satisfies the following conditions:
SiO 2 Al 2 0 3 CaO MgO (Fe 2 O 3 +FeO) Na 2 O K 2 O TiO 2
K in 0.5% 1% 2% 2% 2.5% 3% 3% 3%
f n 1% 2% 4% 4% 5% 6% 6% 6%
the homogenized ore raw materials meeting the conditions are matched with the electric melting tank furnace, continuous basalt fibers can be stably and efficiently controlled, the strength dispersion of the precursor is smaller than or equal to 3%, the elastic modulus dispersion is smaller than or equal to 3%, the wiredrawing yield is larger than or equal to 92%, wiredrawing operation with the specification of 7-22 mu m is realized, the wiredrawing operation is suitable for 400-2400-hole bushing operation, the wiredrawing yield is larger than or equal to 92%, the service life of the furnace is 3-4 years, the service life of the bushing is 6-8 months, the strength of the precursor is 2200-3300 MPa, the elastic modulus is 86-96 Pa, and ten thousand tons of basalt fibers can be produced annually.
When the method is used specifically, the granularity of the homogenized basalt ore is controlled to be 1-3mm, and the homogenization method can be a conventional mechanical stirring or pneumatic (air flow) mixing method. The homogenized batch is 140-210 tons (the batch is calculated by adding 20-30 times of the model of the kiln and the daily output). After the homogenization process is finished, five samples are randomly sampled, each sample is 5-10 Kg, and the samples are crushed and ground until the granularity is less than or equal to 70. Fully stirring and homogenizing each obtained sample in a small mechanical stirring or ball milling stirrer, randomly taking five subsamples of the fully homogenized five samples, testing chemical components of the subsamples, and measuring SiO of the subsamples 2 、Al 2 O 3 、CaO、MgO、Fe 2 O 3 、FeO、 TiO 2 、K 2 O、Na 2 O、MnO 2 The content of (a).According to a calculation formula
Figure RE-GDA0003734818200000101
Where A is in A certain oxide representing the ith sub-sample in the nth sample, for example: SiO 2 2 The weight percentage of CaO, etc.,
Figure RE-GDA0003734818200000102
denotes the average value of a certain oxide in the n-th sample, K in The dispersion coefficient of an oxide of the ith subsample in the nth sample is shown.
Calculating the homogenization accuracy requirement (K) of the five subsamples according to the formula in ) The following were used:
oxide compound SiO 2 Al 2 0 3 CaO MgO Fe 2 O 3 +FeO Na 2 O K 2 O TiO 2
K in 0.5% 1% 2% 2% 2.5% 3% 3% 3%
And if the homogenized chemical composition test result of the subsample does not meet the requirement, continuing the homogenization process until the homogenized chemical composition test result is qualified.
For five samples (each containing five subsamples) the calculation:
Figure RE-GDA0003734818200000111
where B represents the average of a certain oxide in five samples, f n The dispersion coefficient of an average value of a certain oxide in the nth sample is expressed. The test results of the above samples and sub-samples were homogenized to pass if the following requirements were met:
oxide compound SiO 2 Al 2 0 3 CaO MgO Fe 2 O 3 +FeO Na 2 O K 2 O TiO 2
f n 1% 2% 4% 4% 5% 6% 6% 6%
The calculated data of the average oxide content are as follows:
Figure RE-GDA0003734818200000112
wherein A is in Is an oxide of the ith subsample in the nth sample.
The invention also calculates the discrete coefficients simultaneously:
the discrete coefficient formula is:
Figure RE-GDA0003734818200000113
taking into account a certain sub-sample A in case of sufficient homogenization in And the mean value
Figure RE-GDA0003734818200000114
The difference is not large, here approximately the same value Δ, then:
Figure RE-GDA0003734818200000115
therefore, the number of the first and second electrodes is increased,
Figure RE-GDA0003734818200000116
same as above
Figure RE-GDA0003734818200000117
For the basalt component for wire drawing, the following requirements are satisfied:
SiO 2 ≤60%,Al 2 O 3 ≤20%,CaO≤10%,MgO≤7%,(Fe 2 O 3 +FeO)≤12%, K 2 O≤6%,Na 2 O≤6%,TiO 2 ≤2%。
in this application, K is in Required data substitution: delta SiO 2 ≤3%,ΔAl 2 O 3 ≤2%,ΔCaO≤2%,ΔMgO≤1.4%,Δ(Fe 2 O 3 +FeO)≤3%,ΔK 2 O≤1.8%,ΔNa 2 O≤1.8%,ΔTiO 2 ≤0.6%。
According to the relation between the physical properties and the composition of the glass:
G=K 1 ·SiO 2 +K 2 ·Al 2 O 3 +K 3 ·CaO+K 4 ·MgO+K 5 ·(Fe 2 O 3 +FeO)+K 6 ·K 2 O+K 7 · Na 2 O+K 8 ·TiO 2 and then:
ΔG=K 1 ·ΔSiO 2 +K 2 ·ΔAl 2 O 3 +K 3 ·ΔCaO+K 4 ·ΔMgO+K 5 ·Δ(Fe 2 O 3 +FeO)+K 6 ·ΔK 2 O+K 7 ·ΔNa 2 O+K 8 ·ΔTiO 2 ≤ K 1 ×0.5%SiO 2 +K 2 ×1%Al 2 O 3 +K 3 ×2%CaO+K 4 ×2%MgO+K 5 ×2.5%(Fe 2 O 3 +FeO) +K 6 ×3%K 2 O+K 7 ×3%Na 2 O+K 8 ×3%TiO 2 ≤(K 1 ·SiO 2 +K 2 ·Al 2 O 3 +K 3 ·CaO+K 4 · MgO+K 5 ·(Fe 2 O 3 +FeO)+K 6 ·K 2 O+K 7 ·Na 2 O+K 8 ·TiO 2 )×3%≈G×3%,
in summary, the coefficient of variation of performance G is equal to or less than 3%.
The actual homogenization process comprises the homogenization of a large batch (the scale of tens of tons and hundreds of tons), and the range of ≦ 6% (according to f) can be obtained according to the requirements of the raw material components n Calculation). The forced homogenization of small-batch homogenization and convection homogenization in the kiln can completely realize K in And (d) the corresponding process target of ≦ 3%.
In addition, the uniformity control method can achieve better effect by matching with the electric melting tank furnace designed by the applicant. Specifically, referring to fig. 2, a blocking brick 300 is arranged between the melting tank 101 and the uptake 102, the top of the blocking brick 300 is fixed on the inner wall of the top of the melting tank 101, and the bottom of the blocking brick 300 and the bottom of the melting tank 101 have a preset height for conducting the melt; at least one convection chamber 400 is arranged between the melting tank 101 and the baffle brick 300, and in the embodiment, 2 convection chambers 400 are designed. The convection chamber 400 has a vertically through structure. The blocking brick 300 is used for separating the melting tank 101 and the ascending channel 102, and a liquid flow hole with a certain height and width is formed between the lower part of the blocking brick 300 and the bottom of the melting tank 101 and is used for conducting melt formed by the melted raw materials to flow into the ascending channel 102; this application is through this fender brick 300 structure of convection chamber 400 cooperation that adds for the raw materials is in keeping off the left convection chamber 400 of brick 300 structure inside and outside fully to the convection current dispersion in order to realize homogeneity control.
Referring to fig. 2, 1011 is the feed liquid level and the convection chamber 400 is designed below the feed liquid level 1011 and above the bottom of the block, i.e. the bottom surface of the convection chamber 400 is higher than the bottom surface of the block 300. This convection current room 400 has open-top, middle part cavity portion and bottom opening, and open-top's width and bottom opening's width all are less than the width of middle part cavity portion, make the solution that the material formed can be fully in convection current room 400 homodisperse. Meanwhile, the convection chamber 400 is arranged between the two charging openings, i.e. the convection chamber 400 is not arranged under the charging openings, thereby further ensuring that the internal solution is fully and uniformly dispersed inside and outside the convection chamber 400 in the flowing process.
In actual use, the charging device charges basalt material into the furnace body 100 through the charging port 105, and the basalt material sequentially passes through the melting tank 101 → the blocking brick 300 → the ascending channel 102 → the main material channel 103 → the working chamber 104 (bushing zone); the electric melting control device is used for electrifying the electrode assembly, controlling the transformer to change the power of the electrode assembly according to the temperature information in the furnace fed back by the thermocouple assembly, keeping the temperature in the kiln at 1400-1700 ℃, and fully melting the basalt material into uniform melt.
The device is used by combining an electric melting furnace, further uniformity control is realized through a heat convection area designed by the electric melting furnace and convection and diffusion in the whole liquid flow process of the furnace, and continuous basalt fibers can be prepared and drawn. When in use, the batch of the materials is 1/3 with daily output within 5 tons every time, and multiple times of materials are preferably adopted. Conventional mechanical agitation or pneumatic (air flow) homogenization methods are employed. When the raw material batches are replaced, the proportion and the weight of the batch are recalculated according to the patent requirements. The water content is measured during calculation, and the weight of the dried raw materials is taken as the basis for calculation. In the method, the granularity of the basalt ore is controlled to be 0.5-3 mm, and the method is based on the combination of the method and an electric melting tank furnace process and is suitable for adopting particle raw materials. The granularity is controlled to be 0.5-3 mm, so that raw materials are melted, dust is controlled, and automatic feeding is facilitated.
The homogenization method in this method uses conventional mechanical agitation or aerodynamic (air flow) mixing methods. The two homogenization methods can meet the requirement of homogenization of the particle raw materials, and have mature technology and mature equipment.
The method for controlling the uniformity of the components of the ore raw material for manufacturing the continuous basalt fibers by the tank furnace method is characterized in that the homogenized batch is 140-210 tons (the batch is calculated by 20-30 times according to the model of the furnace and the daily output). The specific calculation method comprises the following steps: and (3) homogenizing the batch (the daily output of the kiln is 20-30). The daily production here is calculated as 21 tons.
The method for controlling the uniformity of the ore raw material components for manufacturing the continuous basalt fibers by the tank furnace method is characterized in that five samples are randomly sampled, each sample is 5-10 Kg, and the samples are crushed and ground until the granularity is less than or equal to 70 after the homogenization process is finished. The purpose is to react the uniformity of the bulk raw materials on the macro (5-10 Kg) level by five samples.
The method for controlling the uniformity of the components of the ore raw material for manufacturing the continuous basalt fiber by the tank furnace method is characterized in that each obtained sample is fully stirred and homogenized in a small-sized mechanical stirring or ball-milling stirrer. Thereby determining the homogeneity of each sample body.
The method for controlling the uniformity of the components of the ore raw material for manufacturing the continuous basalt fiber by the tank furnace method is characterized in that five fully homogenized samples are randomly taken, chemical component test is carried out on the samples, and the SiO of the samples is measured 2 、Al 2 O 3 、CaO、MgO、Fe 2 O 3 、FeO、TiO 2 、K 2 O、Na 2 O、 MnO 2 The content of (a). The homogeneity and content of 5 corresponding oxide reaction subsamples in the subsample were determined. Homogenization accuracy requirement of five subsamples (K) in ) When the above table is satisfied, the sample uniformity meets the requirements. The homogenization result of the subsample can meet the requirements of process judgment.
The above requirements all express the following ideas: the batch homogenization reaches 5-10 kg (five samples) of macro scale homogenization, the precise full homogenization reaches 5-10 g (five samples) of macro scale homogenization, and the content of corresponding oxides is expressed. The microscopic homogenization, i.e. the homogenization at the molecular level, is realized in the electric melting tank furnace through the heat convection area designed in the electric melting tank furnace and the convection and diffusion in the integral night flow process of the furnace. f. of n The uniformity of 5-10 kg in macroscopic scale is expressed. K is in Expresses the precise and sufficient homogenization of 5-10 g (pentagram) in macroscopic scale. B expresses the oxide content of the whole kiln.
The method requires that 1/3 with daily output of less than 5 tons is used for batching in batches each time, and multiple batching is preferably adopted. The uniformity of the macroscopic kiln on the level of 5 tons is realized. A batch of 5 tons or more is a practically feasible batch. Of course, less than 5 tons, it is technically feasible to increase the number of doses.
When the raw material batches are replaced in the method, the proportion and the weight of the batch materials are recalculated according to patent requirements. The stability of the raw material components of each batch is ensured.
In the method, the water content is required to be measured during calculation, and the weight of the dry raw materials is taken as the basis for calculation. Ensuring the accuracy of the actual content of the oxide.
By using the scheme of the application, the process and the quality of continuous basalt fibers can be stably and efficiently produced and controlled by matching with an electric melting tank furnace, the strength dispersion of the precursor is less than or equal to 3%, the elastic modulus dispersion is less than or equal to 3%, the wire drawing yield is greater than or equal to 92%, the wire drawing operation with the specification of 7-22 microns is realized, the process is suitable for the bushing operation with 400-2400 holes, the strength of the precursor is 2200-3300 MPa, the elastic modulus is 86-96 Pa, the wire drawing yield is greater than or equal to 92%, the service life of a kiln is 3-4 years, the service life of the bushing is 4-8 months, and the annual production of ten thousand tons of basalt fibers can be realized.
In addition, the method of the present invention is not limited to be performed in the time sequence described in the specification, and may be performed in other time sequences, in parallel, or independently. Therefore, the order of execution of the methods described in this specification does not limit the technical scope of the present invention.
While the present invention has been disclosed above by the description of specific embodiments thereof, it should be understood that all of the embodiments and examples described above are illustrative and not restrictive. Various modifications, improvements and equivalents of the invention may be devised by those skilled in the art within the spirit and scope of the appended claims. Such modifications, improvements and equivalents are also intended to be included within the scope of the present invention.

Claims (4)

1. A method for controlling the uniformity of an ore raw material for basalt fibers is characterized by comprising the following steps: the method comprises the following steps:
step 1: selecting a plurality of preset ore raw materials, and mixing and homogenizing the selected ore raw materials according to a preset proportion to prepare a primary mixed raw material; the granularity of the primary mixed raw material is 1-3 mm; the mixing method for mixing and homogenizing the raw materials to be preliminarily mixed can be realized by adopting a conventional mechanical stirring method or a material flow mixing method or a pneumatic mixing method;
step 2: taking five samples in the primary mixed raw materials, crushing each sample, and processing into micro powder to form a secondary mixed raw material; wherein each sample is selected in kilogram order;
and 3, step 3: taking five sub-samples in the secondary mixed raw material, and respectively calculating the chemical composition test of each oxide in the sub-samples, wherein the oxide is SiO 2 、CaO、MgO、Al 2 0 3 、Fe 2 O 3 、FeO、Na 2 O、K 2 O or TiO 2 Judging whether homogenization is finished or not according to a chemical component test result; if the chemical component test result does not meet the requirement, repeating the step 1 to the step 3; if the chemical composition test results meet the requirements, homogenization is completed.
2. The method of controlling the uniformity of an ore material for basalt fiber according to claim 1, characterized by comprising: step 3 comprises calculating:
Figure FDA0003584400000000011
wherein A is in An oxide representing the ith (1. ltoreq. i.ltoreq.5) child sample of the nth (1. ltoreq. n.ltoreq.5) sample, the oxide being SiO 2 、CaO、MgO、Al 2 0 3 、Fe 2 O 3 、FeO、Na 2 O、K 2 O or TiO 2
Figure FDA0003584400000000012
Represents the average value of certain oxides in the n (1. ltoreq. n.ltoreq.5) th sample, K in Representing the dispersion coefficient of the ith (1. ltoreq. i.ltoreq.5) subsample in the nth (1. ltoreq. n.ltoreq.5) sample;and each oxide has a dispersion coefficient K of the ith (1. ltoreq. i.ltoreq.5) sub-sample in the nth (1. ltoreq. n.ltoreq.5) sample in Satisfies the following conditions:
Figure FDA0003584400000000013
Figure FDA0003584400000000021
3. the method of controlling the uniformity of an ore material for basalt fiber according to claim 2, characterized by comprising: step 3 also includes: computing
Figure FDA0003584400000000022
B represents the average of certain oxides of five samples, f n A dispersion coefficient representing an average value of an oxide in the n (1. ltoreq. n.ltoreq.5) th sample; and the dispersion coefficient f of the average value of each oxide in the n (1. ltoreq. n. ltoreq.5) th sample n Satisfies the following conditions:
SiO 2 Al 2 0 3 CaO MgO (Fe 2 O 3 +FeO) Na 2 O K 2 O TiO 2 f n 1% 2% 4% 4% 5% 6% 6% 6%
4. the method for controlling the uniformity of an ore material for basalt fiber according to claim 3, characterized by comprising: the average value of an oxide in five samples was further calculated as follows:
Figure FDA0003584400000000023
wherein A is in An oxide of the ith (1. ltoreq. i.ltoreq.5) child sample of the nth (1. ltoreq. n.ltoreq.5) sample,
Figure FDA0003584400000000024
represents the average value of a certain oxide in the n-th (1. ltoreq. n.ltoreq.5) sample.
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