Method for detecting the volatility of an oil bath solution for viscose fibre oil

Abstract

The application discloses a viscose fiber oil agent oil bath solution volatility detection method, which comprises the following steps: mixing viscose fiber oil agent to be detected and deionized water according to a predetermined ratio to prepare an oil bath solution; weighing the oil bath solution with a mass of m, weighing and recording the total mass of the container and the weighed oil bath solution; placing the container into an oven, weighing and recording the total mass of the container and the residue after drying to a constant weight; and calculating the effective volatility rate. The application relates to the technical field of oil agent performance detection, directly takes the oil bath solution actually used in the production field as a detection object, instead of the oil agent pure product which is not in the actual application form, so that the detection result can truly reflect the volatilization behavior of the oil agent in the subsequent drying section, and the blank of the oil bath solution volatility detection in the industry is filled.

Description

Technical Field

[0001] This invention relates to the field of oil performance testing technology, specifically a method for testing the volatility of viscose fiber oil bath solution. Background Technology

[0002] In the viscose staple fiber manufacturing industry, oiling agents are key auxiliary materials for improving the processing performance of viscose fibers and enhancing the final product quality. Oiling agents are typically formulated with a variety of surfactants, with nonionic surfactants as the core component, supplemented by small amounts of anionic antistatic agents and other ingredients. During the oiling process, they can adhere evenly to the fiber surface, imparting good smoothness, cohesion, and antistatic properties to the fibers, ensuring smooth subsequent textile processing. The stability evaluation of oiling agents is directly related to oiling agent selection, formulation optimization, and production quality control, making it a crucial aspect of industry focus.

[0003] However, current industry-specific testing technologies and research systems for the stability of viscose fiber oils mainly focus on evaluating the physicochemical properties of the oil's basic dispersion system. Common testing methods include room temperature storage tests (observing whether the oil exhibits stratification, precipitation, discoloration, etc., after prolonged static storage) and high-temperature stability tests. The core purpose of these technologies is to verify the physicochemical stability of the oil itself during storage, transportation, and initial use, without considering the impact of specific operating parameters in the viscose fiber production process on the oil's performance.

[0004] In actual viscose fiber production processes, the oiling agent is not used directly in its pure form. Instead, it needs to be prepared into an oil bath solution with deionized water in a specific ratio for fiber oiling. After oiling, the fibers immediately enter a drying section at approximately 135-145℃. During this process, the water in the oil bath solution evaporates rapidly, while the effective components of the oiling agent must adhere evenly to and remain on the fiber surface. Existing testing methods focus on the stability of the pure oiling agent, neglecting the interaction between the oiling agent and the solvent (deionized water) in the oil bath solution, as well as the influence of concentration effects on the thermodynamic stability of the oiling agent. In many cases, oiling agents that pass existing pure product stability tests exhibit abnormal volatilization behavior when prepared into an oil bath solution and subjected to actual drying conditions. This means that the effective components of the oiling agent are unnecessarily and excessively lost at high temperatures, not only reducing the actual utilization rate of the oiling agent but also causing the volatilized oil components to condense and adhere to the heat exchanger surface in the drying section, forming a viscous oil deposit.

[0005] This oil buildup frequently clogs heat exchange channels, increasing the frequency of equipment shutdowns for cleaning and the workload of manual maintenance. It also significantly reduces heat exchange efficiency and dramatically increases drying steam consumption, thereby affecting the production efficiency and product quality stability of upstream processes. For oil product manufacturers, because existing testing methods have failed to establish an effective correlation mechanism between the stability of oil bath solutions and the components of oil product formulations, they often lack clear direction in formula optimization, relying heavily on repeated trial and error, which severely restricts the overall technological upgrading of the industry. More importantly, existing high-temperature stability tests and room-temperature storage tests for pure products are completely incapable of predicting these production risks. These issues are often only discovered passively after problems such as oil buildup and abnormal energy consumption occur in actual production, by which time irreparable economic losses have already occurred.

[0006] Therefore, the industry urgently needs a detection method that can reflect the high-temperature volatilization behavior of viscose fiber oils in actual application form (i.e., oil bath solution) to fill the gap in the existing technology for evaluating the volatility of oil bath solutions, and provide a scientific and reliable detection method for oil stability assessment, production risk prediction and precise formulation optimization. Summary of the Invention

[0007] (a) Technical problems to be solved To address the shortcomings of existing technologies, this invention provides a method for detecting the volatility of viscose fiber oil bath solutions. This method solves the technical problem that existing detection methods only evaluate the stability of pure oil products and cannot reflect the actual volatilization behavior of oil bath solutions under actual production drying conditions.

[0008] (II) Technical Solution To achieve the above objectives, the present invention provides the following technical solution: a method for detecting the volatility of viscose fiber oil bath solution, comprising the following steps: (1) Mix the viscose fiber oil to be tested with deionized water in a predetermined ratio and stir evenly at a temperature of 50℃~70℃ to prepare an oil bath solution; (2) Weigh out a mass of m of the oil bath solution, place it in a pre-weighed container, weigh and record the total mass of the container and the weighed oil bath solution; (3) Place the container containing the oil bath solution into an oven and dry it at a temperature of 130°C to 145°C until constant weight. Weigh and record the total mass of the container and the residue after drying to constant weight. (4) Calculate the effective volatile rate according to the following steps: First, based on the mass m of the oil bath solution and the predetermined ratio described in step (1), calculate the mass of viscose fiber oil contained in the oil bath solution and record it as W; Then, based on the mass recorded in steps (2) and (3), calculate the mass of the residue in the container after drying to constant weight, and record it as M; Finally, the effective evaporation rate is calculated using the formula: Effective evaporation rate = (W - M) / W × 100%.

[0009] In some embodiments, in step (1), the deionized water is first heated to 60°C~70°C, then mixed with the viscose fiber oil to be tested, and stirred with a magnetic stirrer until the solution is uniform, without layering and without oily particles.

[0010] By preheating deionized water and using magnetic stirring, the actual configuration conditions of the oil bath in the production site can be more closely simulated, ensuring that the oil is fully dispersed in the solution and avoiding detection errors caused by insufficient dissolution.

[0011] In some embodiments, in step (1), the prepared oil bath solution is a homogeneous solution that is visually free of stratification and oily particles.

[0012] Using visual uniformity as the criterion for determining the completion of solution preparation is intuitive and simple to operate, and can ensure the consistency of the samples to be tested, making the test results comparable.

[0013] In some embodiments, in step (2), the container is a flat weighing bottle with a ground glass cap, and the constant weight standard of the weighing bottle is that the weight difference between two weighings does not exceed 0.0003g.

[0014] Flat weighing bottles have a large evaporation area and good thermal conductivity, which is conducive to the rapid evaporation of moisture during the drying process. At the same time, the ground glass cap can be removed during drying to facilitate the escape of water vapor. When the cap is closed during cooling and weighing, it can prevent moisture absorption from affecting the weighing accuracy. The constant weight standard that the weight difference between two weighings does not exceed 0.0003g ensures the high stability of the container's own mass and provides a reliable benchmark for subsequent precision weighing.

[0015] In some embodiments, in step (2), the mass of the oil bath solution weighed is 10~11g, and the weighing accuracy is 0.0001g.

[0016] Choosing this mass range ensures that the amount of effective components in the sample meets the analytical sensitivity requirements, keeps the drying time within a reasonable range, and ensures that the analytical balance accuracy of 0.01 g guarantees the significant digits of the volatility calculation results.

[0017] In some embodiments, in step (3), the oven is preheated for at least 30 minutes before the container containing the oil bath solution is placed in; when placing the containers, the distance between them is not less than 5 cm and they do not contact the inner wall of the oven.

[0018] The preheating oven ensures that the temperature quickly returns to the set value after the sample is placed in, reducing the impact of temperature fluctuations; the specified spacing and avoidance of contact with the inner wall ensure the uniformity of hot air circulation in the oven, so that each sample is heated evenly and the test results are reproducible.

[0019] In some embodiments, in step (3), the condition for determining constant weight is: if the mass reduction between two consecutive weighings does not exceed 0.001g, then constant weight is considered to have been reached; if a mass increase occurs, then the mass of the weighing before the mass increase is used as the basis for calculating M, and the drying process ends.

[0020] In the later stages of high-temperature drying, the water in the oil bath solution has basically evaporated, and the mass of the residue tends to stabilize. However, the mass may rebound due to factors such as slight oxidation and weight gain. At this time, the previous weighing value can be used as the standard to avoid underestimating the effective evaporation rate.

[0021] In some embodiments, in step (4), two parallel samples are set for testing, and the effective volatility is the average of the calculation results of the two parallel samples.

[0022] The dual-parallel design meets the general requirements of quantitative chemical analysis, effectively evaluates the precision of the test results, and eliminates random errors.

[0023] In some embodiments, the method further includes the following steps: comparing the calculated effective evaporation rate with a preset threshold, and when the effective evaporation rate exceeds the preset threshold, determining that the oil agent poses a risk of causing oil buildup in the heat exchanger during viscose fiber production.

[0024] By using preset thresholds, rapid risk warnings can be achieved, enabling production enterprises to identify high-risk oils before they enter the plant or are used, thus avoiding potential equipment pollution and increased energy consumption caused by excessive volatilization.

[0025] In some embodiments, the viscose fiber oil to be tested is an oil with multiple candidate formulations, and the volatility detection method further includes the following steps: comparing the effective volatility corresponding to each of the candidate formulations, and selecting the formulation corresponding to the effective volatility that meets the preset conditions as the production oil formulation based on the comparison results.

[0026] This method provides a clear quantitative basis for the screening and optimization of oil formulations. Researchers can quickly locate the optimal formulation based on the effective volatility, or know the direction of formulation adjustment (i.e., whether to increase or decrease the HLB value), which significantly improves the efficiency of formulation development.

[0027] (III) Beneficial Effects The beneficial effects of this invention are: The test directly uses the oil bath solution actually used on the production site, rather than the pure oil product that is detached from its actual application form. This allows the test results to truly reflect the volatility behavior of the oil in the subsequent drying process, filling the gap in the industry for testing the volatility of oil bath solutions.

[0028] By introducing effective volatility as a quantitative evaluation index for oil stability, the volatility of the solution is incorporated into the evaluation system for oil stability. This breaks through the limitations of traditional methods that only focus on the stratification, discoloration, and thermal weight loss of pure products, and expands the evaluation dimension from "pure product stability" to "application-state volatility".

[0029] Using the temperature of the drying section as the testing condition and simulating the on-site oil bath preparation temperature and method, the volatilization behavior in the test was highly consistent with the actual production, and the test results have direct guiding significance for production.

[0030] Based on the effective volatility value, the risk of oil deposits in heat exchangers caused by oil during production can be directly predicted, transforming quality control from "passive handling" to "proactive prevention." This can help avoid production losses, reduce equipment cleaning costs and downtime, and ensure continuous production efficiency.

[0031] The entire testing process involves only standard weighing and drying equipment, requiring no complex or expensive specialized instruments. The simple operating steps facilitate rapid adoption by various companies across the industry. The calculation of the effective volatilization rate is clear and intuitive, allowing even non-professionals to quickly grasp and interpret it.

[0032] The correlation between effective volatility and HLB value provides oil manufacturers with a clear direction for formula adjustment. Researchers can determine whether to reduce or increase the HLB value of the formula based on the test results of effective volatility, thereby making targeted adjustments to the component ratio, accelerating the development of new products, and achieving synergistic cost reduction and efficiency improvement in upstream and downstream industries.

[0033] Experimental results show that the relative standard deviation (RSD) of this method is less than 5% in 12 parallel tests, which fully meets the precision requirements of laboratory quantitative detection methods. The data is stable and reliable, and can meet the dual needs of production quality control and laboratory research. Attached Figure Description

[0034] Figure 1 This is a schematic diagram of the detection process of the present invention. Detailed Implementation

[0035] To better understand the above technical solutions, exemplary embodiments of the present invention will be described in more detail below with reference to the accompanying drawings. Although exemplary embodiments of the present invention are shown in the drawings, it should be understood that the present invention can be implemented in various forms and should not be limited to the embodiments set forth herein. Rather, these embodiments are provided so that the present invention can be understood more clearly and thoroughly, and that the scope of the present invention can be fully conveyed to those skilled in the art.

[0036] Example 1

[0037] Please see Figure 1 This invention provides a technical solution: a method for detecting the volatility of viscose fiber oil bath solution, the specific steps of which are as follows: Step (1): Preparation of oil bath solution.

[0038] Accurately weigh a certain amount of the viscose fiber oil to be tested, accurate to 0.0001g. Determine the concentration based on the actual production site conditions or testing requirements; this concentration is the predetermined ratio. Measure the required volume of deionized water and heat it to 60℃~70℃ (e.g., 65℃). Then, add the preheated deionized water and the weighed oil to a clean container. Place the container on a magnetic stirrer, add a clean stir bar, and start stirring at medium speed for about 5 minutes, until the solution is visually observed to be free of layering and oily particles, and appears uniformly transparent or semi-transparent; this is the oil bath solution.

[0039] Step (2): Transfer and weighing of oil solution.

[0040] Take a pre-weighed flat weighing bottle (70×35mm, with a ground glass cap). The standard for constant weight of this weighing bottle is: after drying in an oven at 135℃, cool to room temperature in a desiccator, weigh it using an analytical balance (accuracy 0.0001g), and the difference between two weighings should not exceed 0.0003g. Record the accurate mass of the weighing bottle after constant weight. Using the direct weighing method, accurately transfer about 10~11g of the oil bath solution prepared in step (1) using a pipette or dropper, place it in the weighing bottle, immediately cover it with the ground glass cap, accurately weigh it on an analytical balance, and record the total mass of the weighing bottle and the transferred oil bath solution. Thus, the mass m of the weighed oil bath solution is obtained.

[0041] Step (3): Dry and weigh.

[0042] Turn on the oven in advance, set the temperature to 135℃, and preheat for at least 30 minutes to ensure that the temperature inside the oven is stable and uniform. Remove the ground glass cap from the weighing bottle containing the oil bath solution in step (2) (the cap can be placed in the oven to dry, but not on the bottle). Place the weighing bottles evenly on the oven partition, with a distance of not less than 5cm between the bottles, and none of the weighing bottles should touch the inner wall of the oven. Close the oven door and start drying. During the drying process, take out the weighing bottle at regular intervals, put on the ground glass cap, and place it in the desiccator to cool to room temperature before weighing. The first sampling can be carried out 2 hours after drying, and the interval can be adjusted appropriately according to the weight loss. When the mass reduction of two consecutive weighings does not exceed 0.0010g, it is considered to have reached constant weight, and drying is stopped. If a certain weighing shows that the mass has increased compared to the previous one, the previous weighing value is used as the drying endpoint, and the total mass of the weighing bottle and the residue at this time is recorded.

[0043] Step (4): Calculation of effective volatile rate.

[0044] First, calculate the effective oil content W in the oil bath solution: Based on the predetermined ratio of oil to deionized water in step (1), and combined with the oil bath solution mass m obtained in step (2), calculate the corresponding oil content W. For example, if the concentration is C (g / L), the volume of the solution taken can be indirectly converted from mass m and density or directly calculated according to the ratio, then W = (oil content / total solution content) × m. The calculation method here is the conventional operation in this field. Next, calculate the residue mass M: The difference between the total mass of (container + solution) recorded in step (2) and the total mass of (container + residue) recorded in step (3) is the residue mass M after drying (the weight of the container itself has been deducted because the constant weight of the weighing bottle is known). Then calculate the effective evaporation rate according to the formula = (W - M) / W × 100%, expressed as a percentage.

[0045] In this embodiment, two parallel samples are set up, and the final effective volatilization rate is the average of the two calculation results.

[0046] This embodiment provides a method for detecting the volatility of viscose fiber oil bath solutions. By simulating the actual preparation method of the oil bath solution and the drying temperature, the effective volatility of the oil directly reflects the proportion of loss of the effective components during the drying process. The underlying reason for this loss proportion is directly related to the hydrophilic-lipophilic balance (HLB) value of the oil formulation system. When the HLB value of the oil formulation deviates from the optimal range best suited for the production conditions, whether it deviates in the direction of excessive lipophilicity, leading to significant volatilization of low-boiling-point lipophilic components at high temperatures, or deviates in the direction of excessive hydrophilicity, leading to increased loss of effective components due to water molecules binding with water molecules and being carried away by water vapor, it will manifest as an increase in the effective volatility value. Therefore, this method quantifies the stability and high-temperature volatilization behavior of oil emulsions, which are difficult to evaluate quickly and accurately using conventional methods, into a directly comparable effective volatility index. The test results show a clear positive correlation with the degree of oil buildup on the surface of the heat exchanger in the drying section of the production line and the non-productive loss of oil. Therefore, it can be used to predict the risk of oil contamination and the level of oil loss in actual production, and provide a clear direction for oil production enterprises to optimize their formulations—that is, by adjusting the hydrophilic and lipophilic ratio of each component in the formulation, the HLB value of the system tends to the suitable range that minimizes the effective volatility. This method not only fills the gap in existing technologies that only evaluate the stability of pure oil products, but also achieves a direct leap from laboratory testing to production risk prediction. It is simple to operate, reliable in results, and has significant application value.

[0047] Example 2

[0048] Based on Example 1, this embodiment further provides a method for predicting the stability risk of oil agents using the effective volatility.

[0049] The effective volatile rate calculated in step (4) is compared with a preset threshold. This preset threshold is a critical value determined based on actual production experience or through statistical data analysis to distinguish whether the oil agent will generate an unacceptable risk of oil stain accumulation during production. When the effective volatile rate exceeds the preset threshold, it is determined that the oil agent poses a risk of causing oil stain accumulation in the heat exchanger during viscose fiber production; when the effective volatile rate does not exceed the preset threshold, it is determined that the volatile stability of the oil agent meets the production requirements and can be used normally.

[0050] This embodiment extends the detection method from simple numerical measurement to a clear risk assessment stage, enabling manufacturers to complete risk screening before oils are inspected upon arrival at the factory or before they are used. High-risk oils can be replaced or their formulations adjusted in a timely manner to prevent them from entering the production line and causing equipment pollution and energy loss.

[0051] Example 3

[0052] Based on Example 1, this embodiment further provides a method for screening and optimizing oil formulations using effective volatility.

[0053] When the viscose fiber oil to be tested is an oil with multiple candidate formulations, steps (1) to (4) of Example 1 are performed on each candidate formulation to obtain the effective volatility corresponding to each candidate formulation. Then, the effective volatility corresponding to each candidate formulation is compared, and the formulation with the effective volatility that meets the preset conditions is selected as the oil formulation for production based on the comparison results. The preset conditions include, but are not limited to: the lowest effective volatility, the effective volatility being lower than a certain preset threshold, or the effective volatility falling into a certain preset optimal range.

[0054] This embodiment provides a clear quantitative basis for screening oil formulations. When developing new formulations or optimizing existing ones, researchers no longer need to rely on repeated trial-and-error experiments or cumbersome HLB value measurements. They can quickly determine the formulation with the best overall volatility stability simply by testing the effective volatility of different candidate formulations.

[0055] To further verify the technical effects of the present invention and its advantages over the prior art, the applicant conducted systematic experimental verification, which is described in detail below through multiple experimental examples.

[0056] Experimental Example 1 Volatility testing of oil bath solutions with different formulations This experimental example uses the method of Example 1 of the present invention to test the volatility of oil bath solutions of various viscose fiber oils with different components and ratios, in order to examine the method's ability to distinguish between different oil samples.

[0057] The information for the tested oil samples is as follows. The various components involved in the formulations of the following samples are all commercially available surfactants or functional additives commonly used in viscose fiber oils in this field. For ease of identification, they are referred to by codes: Sample 1: An oil preparation made by compounding component A and component B in a mass ratio of 4:6; wherein component A is a nonionic surfactant and component B is an anionic antistatic agent; Sample 2: An oil preparation made by compounding component C and component D in a mass ratio of 6:4; wherein, both component C and component D are nonionic surfactants, and their hydrophilic-lipophilic balance values ​​(HLB values) are different; Sample 3: An oil formulation composed of component E and component F in a mass ratio of 7:3; wherein, both component E and component F are nonionic surfactants, and their HLB values ​​are different; Sample 4: An oil-based agent composed of a single component G; wherein component G is a nonionic surfactant; Sample 5: A commercially available viscose fiber oiling agent, whose main component is a nonionic surfactant compound system; Sample 6: An oil preparation made by compounding component H and component I in a mass ratio of 4:6; wherein, both component H and component I are nonionic surfactants and have different HLB values; Sample 7: An oil preparation made by compounding component J and component K in a mass ratio of 4:6; wherein, component J and component K are both nonionic surfactants and have different HLB values.

[0058] Each oil sample was prepared into two concentrations of oil bath solution: 7 g / L and 9 g / L. During preparation, deionized water was preheated to 65°C and the solution was magnetically stirred until homogeneous.

[0059] The testing procedures were strictly followed according to Example 1, with the oven temperature set at 135°C. Two parallel samples were prepared for each sample, and the average effective volatilization rate was calculated. The test results are shown in Table 1.

[0060] Table 1. Results of volatility test of oil bath solutions with different formulations of oil. As shown in Table 1, the method of this invention can significantly distinguish the high-temperature volatility of different formulations of oils in oil bath solution. The effective volatility of each sample ranges widely, demonstrating good differentiation. Specifically, samples 2 and 3 have relatively low effective volatility, while sample 7 has an abnormally high effective volatility, especially approaching 20% ​​at a concentration of 9 g / L. This indicates that nearly one-fifth of the effective components of this formulation were abnormally lost under simulated drying conditions. This result proves that the method of this invention has excellent differentiation and identification capabilities for oils with different formulation systems.

[0061] Experimental Example 2: Precision Verification of the Method of the Invention To verify the reproducibility and precision of the method of this invention, sample 4 (G single-component oil agent) was used as the subject, and multiple parallel tests were performed continuously at a concentration of 7 g / L. Each test involved independently prepared oil bath solutions and independently sampled, strictly following the steps in Example 1. A total of 12 independent tests were completed, and the results are shown in Table 2.

[0062] Table 2. Repeatability test data of the method of the present invention (sample 4, 7 g / L) Statistical analysis showed that the average effective volatility of the 12 tests was 2.18%, the standard deviation was 0.10%, and the relative standard deviation (RSD) was 4.37%. The RSD being less than 5% indicates that the method of this invention has excellent precision, fully meets the general requirements for reproducibility of results in laboratory quantitative detection methods, and can satisfy the high standards required for stable and reliable detection data in production quality control.

[0063] Experiment Example 3: Production Verification - Effects of Different Oiling Agents on Fiber Oil Content and Oiling Agent Consumption To verify the direct correlation between the effective volatile matter rate measured by the method of this invention and actual production performance, a 30-day follow-up verification was conducted on a continuous viscose staple fiber production line. The process parameters of this production line (spinning type, oiling equipment, drying section operating temperature 135-145℃) were kept constant throughout the process, producing ordinary fibers of the same specification (1.33 dtex × 38 mm). Only two different formulations of oiling agents were used successively: in the first stage, a mixed oiling agent was used, consisting of commercially available oiling agent A and sample 6 mixed in a certain proportion (sample 6 component accounted for 40%, and commercially available oiling agent A component accounted for 60%); in the second stage, another commercially available oiling agent, code JK, was used. During the production process, the fiber oil content was monitored multiple times daily, and the average monthly oiling agent consumption per ton of fiber was calculated. Some production data are shown in Table 3.

[0064] Table 3 Comparison of oil content and oil consumption per unit of fiber produced by different oiling agents As shown in Table 3, the two oiling agents achieve identical oiling effects on the fibers, with an average oil content of 0.31% in both finished fibers, eliminating the interference of different oiling agent consumption due to variations in fiber oiling rates. However, when using the mixed oiling agent containing component 6 of the sample, the oiling agent consumption per ton of fiber is as high as 4.2 kg, while when using the JK oiling agent, the consumption is only 3.7 kg, a difference of approximately 13.5%. Under the premise of the same oil content, the excess oiling agent will inevitably enter the environment in the form of gaseous volatilization or liquid oil mist, eventually condensing and adhering on the heat exchanger surface to form oil scale, and being directly discharged into the waste gas treatment system. This result is highly consistent with the trend of higher effective volatilization rate of sample 6 measured in the method of this invention, strongly demonstrating that the effective volatilization rate index can accurately predict the oiling agent consumption level of the production line and the potential risk of equipment oil scale.

[0065] Experimental Example 4: Comparison of the method of the present invention with existing methods for testing the high-temperature stability of pure products To highlight the substantial advancements of this invention, a typical high-temperature stability testing method for pure products in the prior art was used to compare the thermal stability of components A and B in Sample 1 and components J and K in Sample 7. The testing conditions were as follows: each pure oil component sample was heated in an oven at 105℃, 135℃, 140℃, and 150℃ for 2 hours, and the changes in oil content and volatility were measured. Simultaneously, the effective volatilization rate of the oil bath solutions (9 g / L) prepared from the two compound oils of Sample 1 and Sample 7 was tested using the method of this invention. The comparison results are shown in Table 4.

[0066] Table 4 Comparison of high-temperature stability data of the pure product and volatility data of the oil bath solution of this invention As shown in Table 4, the high-temperature stability data of pure products indicate that components J and K exhibit very low volatilization rates at all temperatures. Particularly at 135℃, J volatilizes by only 0.12% and K by only 0.72%, even surpassing the performance of pure components A and B. According to existing industry standards, the high-temperature resistance of the oil formulation composed of J and K is fully qualified and even considered superior to that of the oil formulation composed of A and B. However, when testing the oil bath solution prepared from these two compound oil formulations using the method of this invention, the effective volatilization rate of sample 7 reached as high as 19.77%, almost 2.6 times that of sample 1 (7.58%). This result profoundly reveals the fundamental flaw of existing pure product testing methods: the thermal stability of oil formulations in their pure state cannot reflect their true volatilization behavior in solution state and under operating temperatures, because complex factors such as solvation effects, inter-component interactions, and water vapor entrainment are completely ignored in pure product testing. In actual production lines, these very factors cause a large amount of volatilization in the oil formulated from components J and K, which performs well in pure product testing, resulting in serious problems such as frequent heat exchanger blockage and a sharp increase in energy consumption. The method of this invention directly addresses this "real-world application state" for evaluation, thus accurately predicting and distinguishing the actual production performance of different oils, filling a significant gap in existing technology, and having significant implications for technological advancement in the industry.

[0067] In summary, the method for detecting the volatility of viscose fiber oil bath solutions provided by this invention has a complete and rigorous technical solution. Through specific combinations of steps and parameter control, it achieves precise quantification of the high-temperature volatilization behavior of the oil under simulated production conditions. Experimental data fully demonstrates that this method not only has high precision and good discrimination, but also that the test results are highly consistent with the actual performance of the production line. It can effectively predict the risk of oil residue accumulation during the use of the oil and guide the screening and optimization of oil formulations. This invention fundamentally changes the current situation where the stability evaluation of oil is divorced from practical applications, providing the industry with a simple, reliable, and highly valuable new detection method for widespread application.

[0068] In the description of this specification, the terms "one embodiment," "some embodiments," "embodiment," "example," "specific example," or "some examples," etc., refer to specific features, structures, materials, or characteristics described in connection with that embodiment or example, which are included in at least one embodiment or example of the present invention. In this specification, the illustrative expressions of the above terms do not necessarily refer to the same embodiment or example. Furthermore, the specific features, structures, materials, or characteristics described may be combined in any suitable manner in one or more embodiments or examples. Moreover, without contradiction, those skilled in the art can combine and integrate the different embodiments or examples described in this specification, as well as the features of different embodiments or examples.

[0069] 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 modifications, alterations, substitutions and variations to the above embodiments within the scope of the present invention.

Claims

1. A method for detecting the volatility of viscose fiber oil bath solution, characterized in that, Includes the following steps: (1) Mix the viscose fiber oil to be tested with deionized water in a predetermined ratio and stir evenly at a temperature of 50℃~70℃ to prepare an oil bath solution; (2) Weigh out a mass of m of the oil bath solution, place it in a pre-weighed container, weigh and record the total mass of the container and the weighed oil bath solution; (3) Place the container containing the oil bath solution into an oven and dry it at a temperature of 130°C to 145°C until constant weight. Weigh and record the total mass of the container and the residue after drying to constant weight. (4) Calculate the effective volatile rate according to the following steps: Based on the mass m of the oil bath solution and the predetermined ratio described in step (1), calculate the mass of viscose fiber oil contained in the oil bath solution and record it as W; Based on the mass recorded in steps (2) and (3), calculate the mass of the residue in the container after drying to constant weight, and denot it as M; Calculate the effective volatility using the following formula. Effective evaporation rate = (W - M) / W × 100%.

2. The method for detecting the volatility of viscose fiber oil bath solution according to claim 1, characterized in that, In step (1), the deionized water is first heated to 60°C~70°C, then mixed with the viscose fiber oil to be tested, and stirred with a magnetic stirrer until the solution is uniform, without layering and without oily particles.

3. The method for detecting the volatility of viscose fiber oil bath solution according to claim 1, characterized in that, In step (1), the prepared oil bath solution is a homogeneous solution that is visually free of layering and oily particles.

4. The method for detecting the volatility of viscose fiber oil bath solution according to claim 1, characterized in that, In step (2), the container is a flat weighing bottle with a ground glass cap, and the constant weight standard of the weighing bottle is that the weight difference between two weighings does not exceed 0.0003g.

5. The method for detecting the volatility of viscose fiber oil bath solution according to claim 1, characterized in that, In step (2), the mass of the oil bath solution weighed is 10~11g, and the weighing accuracy is 0.0001g.

6. The method for detecting the volatility of viscose fiber oil bath solution according to claim 1, characterized in that, In step (3), the oven is preheated for at least 30 minutes, and then the container containing the oil bath solution is placed in it. When placing the containers, the distance between them is not less than 5 cm and they do not contact the inner wall of the oven.

7. The method for detecting the volatility of viscose fiber oil bath solution according to claim 1, characterized in that, In step (3), the condition for determining constant weight is: if the decrease in mass between two consecutive weighings does not exceed 0.001g, then constant weight is considered to have been reached; if there is an increase in mass, then the mass of the weighing before the increase in mass is used as the basis for calculating M, and the drying process ends.

8. The method for detecting the volatility of viscose fiber oil bath solution according to claim 1, characterized in that, In step (4), two parallel samples are set up for testing, and the effective volatility is the average of the calculation results of the two parallel samples.

9. The method for detecting the volatility of viscose fiber oil bath solution according to claim 1, characterized in that, It also includes the following steps: The calculated effective volatile rate is compared with a preset threshold. When the effective volatile rate exceeds the preset threshold, it is determined that the oil agent poses a risk of causing oil buildup in the heat exchanger during viscose fiber production.

10. The method for detecting the volatility of viscose fiber oil bath solution according to claim 1, characterized in that, The viscose fiber oil to be tested is an oil with multiple candidate formulations. The volatility detection method further includes the following steps: comparing the effective volatility of each candidate formulation, and selecting the formulation with the effective volatility that meets the preset conditions as the production oil formulation based on the comparison results.

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