Method for the manufacture of a spinning finisher for treating spiders and yarn

BE1033272A1Pending Publication Date: 2026-07-31VERTEXCO NV
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Patent Information

Authority / Receiving Office
BE · BE
Patent Type
Applications
Current Assignee / Owner
VERTEXCO NV
Filing Date
2024-12-30
Publication Date
2026-07-31
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Description

BE2024 / 5966 2 affect. In addition, there is also thermal instability. Stirring and the exothermic reaction between the acid alkyl phosphate and potassium hydroxide can lead to temperature increases in the solution. This can have a negative influence on the stability of the acid alkyl phosphate, resulting in degradation products that reduce the efficacy of the agent. Both factors ultimately cause the quality and performance of the fibers to be compromised. It is therefore essential to find a solution that offers stable and controlled pH maintenance. A third aspect is that partial neutralization ensures that the product remains acidic, making it unsafe and environmentally unfriendly. It contains harmful substances that pose health and environmental risks. The present invention aims to find at least a solution for some of the aforementioned problems or disadvantages. The purpose of the invention is to provide a method which eliminates these disadvantages.15 SUMMARY OF THE INVENTION In a first aspect, the invention concerns a method for making a spin finishing agent in conclusion 1. The spin finishing agent comprises a mixture of fatty acid-based alkoxylates, demineralized water, biocides, amphiphilic substances, a primary base, a secondary base, and organophosphates. The method involves mixing the components. Subsequently, these are stabilized by a two-stage neutralization process. Advantages of this invention include precise pH control, improved thermal stability, and consistent product quality, even at high temperatures. The combination of organophosphate salts and a balanced pH promotes adhesion to fibers and prevents unwanted side reactions, resulting in improved fiber quality and durability. This spin finishing agent offers long-lasting protection of fibers, resulting in improved service lives and mechanical properties of the treated materials. Further preferred forms of the method can be found in conclusions 2 to 8.30 In a second aspect, the invention concerns a spin finishing agent designed to improve and stabilize polymer / fiber filaments after spinning, with effective prevention of NOx fading and yellowing. Due to the presence of two different bases, a product is obtained that is neutral for use, thus safe to use. While it becomes more acidic during use, which ensures better performance. Further preferred forms of the spin finishing agent can be found in conclusions 10 to 15. 2024 / 5966 BE2024 / 5966 3 DETAILED DESCRIPTION The term 'spin finisher' refers in the present invention to a spin finishing agent used in the treatment of fibres and yarns. This agent5 contains various components, including fatty acid-based alkoxylates, demineralized water, acid organophosphates, biocides, amphiphilic substances and two different bases, which contribute to the final properties of the spin finisher.10 In the present invention, the term 'fatty acid-based alkoxylate' refers to a compound with a structure of the formula R1-CO-(EO)m-(PO)nH, where R1 is an alkyl chain with 1-25 carbon atoms, which may be linear or branched and may contain one or more double bonds. EO stands for an ethylene oxide unit and PO is a propylene oxide unit. The integers indicate the number of ethylene oxide and propylene oxide units, respectively arranged in blocks with a ratio between 2:1 and 5:1. The term 'demi-water' refers to deionized water that is used as a solvent in the formulation of the spin finishing agent.20 In the current invention, the term 'acid organophosphate' refers to a compound with a structure according to the formula R-O-(EO)xP(=O)(OH)2, where R is an alkyl group with 1-20 carbon atoms, which can be linear or branched and optionally contain one or more double bonds. EO is an ethylene oxide unit andx25 is an integer from 1 to 25.The term 'biocides' refers to chemical substances used to prevent microbial contamination in the spin finishing agent. 30 The term 'amphiphilic substance' refers in the current invention to an amphiphilic compound, such as oleoylsarcosic acid, which supports the chemical balance and stability of the spin finishing agent. Which, due to its chemical properties, has the ability to interact with a polar or non-polar medium. 35 The term 'first base' refers to a first basic compound used in the two-step pH adjustment process. In a specific formulation, it has a boiling point lower than the operating temperature. 2024 / 5966 BE2024 / 5966 4 The term 'second base' refers to a second basic compound used in the two-step pH adjustment process, which differs from the first base. Dieineenbezekerdeuitvoeringsvormeen kookpuntheftdie hogerligt dande gebruikstemperatuur.5 The term 'intermediate pH' refers to the intermediate pH level reached during the first step of the pH adjustment process, usually set to a value between 3 and 6, preferably at 5 at 20°C. 10 The term 'final pH' refers to the final pH level reached after the second step of the pH adjustment process, set to a value between 6 and 8, preferably at 7.4 at 20°C. The term 'viscosity' refers to the measure of a fluid's resistance to deformation and flow, with an estimated value of 200 mPa·s for the spin finishing agent. The term 'density' refers to the mass per unit volume of the spin finishing agent, with a value of approximately 1.1 g / cm³. The term 'dry matter content' refers to the percentage of solids in the spin finishing agent, with a minimum value of 70 m%. The term 'reaction vessel' refers to the vessel in which the mixing and pH adjustment processes take place, equipped with stirring and pumping mechanisms to guarantee uniform mixing and pH control.The term 'stirring device' refers to the stirring apparatus used in the reaction vessel, consisting of at least one stirring element on a stirring rod to achieve uniform mixing of the components. The term 'external pump' refers to the external pump used to ensure uniform distribution and mixing of the components within the reaction vessel, which contributes to accurate pH control. A specific component, expressed as a percentage of the total mass of the mixture or solution in which the component is located. It is calculated by dividing the mass of the component in question by the total mass of the system, and multiplying the result by 100. This unit is used to accurately and simply describe the relative quantity of a substance in relation to the total. Unless otherwise defined, all terms used in the description of the invention, including technical and scientific terms, have the meaning as they are generally understood by the expert in the technical field of the invention.For a better assessment of the description of the invention, the following terms are explicitly explained. 15 quantity, a parameter, a duration or moment, and the like, then 20 variations are meant of + / - 20% or less, preferably + / - 10% or less, more preferably + / - 5% or less, even more preferably + / - 1% or less, and even more preferably + / - 0.1% or less than the cited value, insofar as such variations apply to the described invention. Here, however, 25 inclusive or open terms must indicate the presence of what follows, and which do not exclude or prevent the presence of other components, features, elements, members, steps, known from or described in the standard of technology. In a first aspect, the invention comprises a method for manufacturing a spinning finishing agent, suitable for treating fibres and yarn.35 2024 / 5966 BE2024 / 5966 6 In a further execution form, the invention comprises a method for manufacturing a spinning finishing agent comprising 10-80 m% of a fatty acid-based alkoxylate, at least 10 m% demineralized water,0.1-10m% of an acid organophosphate, 0.1-1m% biocides and 0.1-2m% of an amphiphilic substance, 0.1-2m% of a first base and 0.5-2m% of a second base.5 In a further form of implementation, the invention comprises a method for manufacturing a spin finishing agent suitable for treating fibers and yarns. The spin finishing agent comprises 10-80m% of a fatty acid-based alkoxylate, at least 10m% demineralized water, 0.1-10m% of an acid organophosphate, 0.1-1m% biocides and 0.1-2m% of an amphiphilic substance, 0.1-2m% of a first base and 0.5-2m% of a second base. The method comprises mixing of the fatty acid-based alkoxylate, demineralized water, the acid organophosphate, biocides and the amphiphilic substance. The second step is a two-stage pH increase where the pH is first increased to an intermediate pH[3-6] with the first base, followed by a second pH increase to a final pH of[6-8] with the second base. Whereby the second base differs from the first base. In one aspect of the invention, a spin finishing agent is presented which20 makes use of a two-stage pH increase process.This process makes it possible to accurately control and stabilize the pH value of a spin finishing agent, which is crucial for improving the efficiency and effectiveness of the fiber finishing process. The spin finishing agent is carefully formulated with a combination of amphiphilic substances and organophosphates, which together ensure optimal adhesion properties, particularly on hydrophobic fibers. In summary, this invention offers an advanced approach to improving the quality and durability of polymer fibers through a carefully controlled pH elevation process. The combination of amphiphilic substances and organophosphates in the spin finishing agent, together with the two-stage neutralization process, ensures superior performance in preventing NOx fading and yellowing, while the fibers retain their strength, flexibility, and color. According to a specified form of execution, the invention comprises a method whereby the first base comprises an aqueous solution containing 18 v% NH3 and the second base comprises an aqueous solution containing 85 v% triethanolamine.The first step in the neutralization process involves the use of a solution containing 18% NH3, 2024 / 5966 BE2024 / 5966 7 that lowers the pH to an intermediate value of 5. This step is crucial because it ensures an optimal neutralization reaction between the organophosphate and the first base, which promotes the stability of the agent and ensures that only soluble salts are formed. This prevents the formation of insoluble salts that could impair the performance of the finishing agent.5 In the second step, triethanolamine is added, which further increases the pH to a neutral value of 7.4. This carefully controlled pH setting ensures that the spin finishing agent retains its stability and remains effective in its function. The final pH of 7.4 offers an optimal balance between the stability of the active components and skin friendliness, allowing the agent to be used safely. are used without damaging the fibers. Upon evaporation of water from the spin finishing agent, a slightly more acidic environment is created.This is an important advantage of the two-stage pH raising process, because it promotes better adhesion of the agent to the fibers and prevents NOx fading.15 Furthermore, the slightly acidic environment created during evaporation minimizes pH fluctuations during processing, which ensures consistent performance of the finishing agent and reduces possible damage to the fibers. The use of two different bases, ammonia and triethanolamine, offers precise neutralization and contributes to the desired acidic action after evaporation of the ammonia. Because ammonia has a much lower boiling point than the operating temperature of the spinning finishing agent, it evaporates faster and this leads almost immediately to a reduction in the pH value. This rapid process is crucial for the effective stabilization of the fibers and prevents unwanted chemical reactions such as yellowing.The method in the invention is further optimized by the use of a single reaction vessel for both mixing and pH increase, whereby process variations are minimized and a consistent neutral pH is guaranteed in the final product. This avoids unnecessary pumping and makes the process more efficient. In a design form, the invention describes that the final pH is 7.4 at 20°C. In different configurations, the pH of the spin-finishing agent can vary within a range of 6 to 8. Preferably, the pH lies between 6.5 and 7.5, more preferably between 6.7 and 7.3, even more preferably between 6.8 and 7.2, and most preferably between 7.0 and 7.4. These variations offer flexibility in the application of the spin-finishing agent, depending on the specific requirements of the fiber processing processes. In a preferred configuration, the final pH of the spin-finishing agent is preferably set at 7.4 at 20°C. This results in consistent process outcomes and contributes to the overall reliability and quality of the treated fibers.The choice of a pH of 7.4 is preferably aimed at achieving an optimal balance between the stability of the active components and the skin-friendliness of the spinning finisher. This ensures that the treatment of the fibers is consistent and that their mechanical properties are effectively improved. Preferably, a pH value of 7.4 can be achieved through a carefully controlled neutralization process, in which the choice of a specific mix of bases and acids plays a crucial role. In a more preferred formulation, the spinning finisher can be formulated with a range of substances that contribute to maintaining this pH, whereby the presence of organophosphate salts can be particularly beneficial for the chemical stability of the composition. The preference for a pH of 7.4 lies in the fact that it creates an optimal environment for the active components to perform their functions without damaging the fibers. Furthermore, a pH value of 7.4 at 20°C can preferably ensure improved adhesion of the spinning finisher to the fibers.This can lead to improved resistance to external influences such as contamination and mechanical stress, which ultimately results in a longer fiber lifespan. In a preferred formulation, the spin-finishing agent can also contribute to increased resistance to microbial contamination, because a slightly acidic environment is created upon evaporation, which can further improve the effectiveness of the treatment. Preferably, the spin-finishing agent with a pH of 7.4 can find versatile applications in various industries, ranging from textiles to plastics processing. The consistency and reliability of the pH setting make it possible to deploy the agent widely without the need for frequent adjustments or corrections, which can increase the efficiency of the production process. 30 In a preferred version, the invention describes that the intermediate pH is 5 at 20°C. This pH helps stabilize salts and prevents unwanted precipitation. This contributes to improving the process reliability of the spin finishing agent.Maintaining this intermediate pH is preferably essential to ensure the chemical stability of the spin finishing agent, thereby reducing the risk of unwanted reactions that can lead to precipitation. Moreover, no insoluble salts can be formed which, in addition to precipitating and thus reducing activity, also cause a visual issue. Preferably, this pH value ensures that the reactive components of the spin finishing agent remain in a state that maximizes their effectiveness without the formation of insoluble salts. This increases the reliability of the process, because the risk of blockages or malfunctions due to precipitation in the processing equipment is significantly reduced. More preferably, the intermediate pH lies between 4.5 and 5.5, thereby achieving an optimal balance between stability and reactivity. of the components. Even more preferably, the pH lies between 4.8 and 5.2, which allows for even more refined control over the chemical reactions within the spin finishing agent10.Preference is given to a pH setting that allows the spin finishing agent to adapt to variations in temperature and other environmental factors without compromising stability. Preferably, the pH at lower temperatures should not be higher, preferably between 5.0 and 5.5, while at higher temperatures the pH should preferably be between 4.5 and 5.0, to ensure the consistency of the product. In another preferred design, the intermediate pH setting can contribute to reducing the environmental impact of the spin finishing agent by minimizing the use of additional destabilizing chemicals. This preferably makes the product more environmentally friendly and attractive for sustainability-oriented applications. In a preferred design, the invention will describe a method in which mixing and the two-stage pH increase take place in a single reaction vessel. In the preferred design, the mixing and the two-stage pH increase are carried out in a single reaction vessel, which contributes to a more efficient process.This process can optionally minimize the need for interruptions, thereby achieving a more uniform end product. It is desirable that this approach improves the reliability of the spin finishing agent by ensuring the consistency of the chemical composition. In an even further implementation form, the method will describe that both stirring and pumping take place in the reaction vessel during mixing and the two-stage pH increase. This preferred implementation, in which stirring and pumping take place in the same reaction vessel, can reduce mechanical stress and thus preserve the chemical integrity and effectiveness of the spin finishing agent. The integrated use of stirring and pumping during the two-stage pH increase process reduces potential chemical inconsistencies, which leads to a more homogeneous end product with better stability. 2024 / 5966 BE2024 / 5966 10 The integration of these methods into a single reaction vessel can further contribute to a controlled and uniform distribution of the bases, which prevents the formation of local high concentrations that can lead to the degradation of components.In a preferred configuration, the reaction vessel can provide an optimized environment in which the bases are evenly distributed, which increases the effectiveness of the neutralization process. It is also desirable that the use of a single reaction vessel configuration offers the possibility to monitor and control thermally induced pH changes. This can be particularly beneficial in maintaining a neutral pH value, which is essential for the effectiveness of the spin finishing agent. Furthermore, the controlled environment within the reaction vessel can promote the evaporation of water, which leads to a desirable acidifying action of the agent. In a further preferred design, the configuration of the reaction vessel can be such that it offers an optimal balance between mechanical and chemical processes, resulting in an efficient and consistent production process of the spin finishing agent. Through this approach, the reliability and quality of the end product are further improved, which contributes to the overall performance and durability of the treated fibers.20 In a preferred execution, the process for manufacturing a spin finishing agent includes performing a first pH measurement after the addition of the first base and performing a second pH measurement after the addition of the second base. Performing separate pH measurements after every addition of a base ensures a more controlled environment, which promotes the stability and consistency of the spin finishing agent. Through these separate pH measurements, consistent pH regulation is sought, which increases the effectiveness of the spin finishing agent. 30 In a further preferred procedure, the pH is accurately measured after the addition of the first base, ammonia water, to ensure that it reaches the desired intermediate value of 5. This pH value is crucial for guaranteeing an optimal neutralization reaction between the organophosphate and the first base, which contributes to the stability of the product.By achieving an intermediate pH of 5, the formation of only soluble salts is guaranteed, while the formation of insoluble salts is avoided. 2024 / 5966 BE2024 / 5966 11 In a further preferred version, after the addition of the second base, triethanolamine, a new pH measurement is performed to check whether the pH has reached the desired neutral value of 7.4. This second pH measurement is essential for ensuring consistency in pH regulation and for optimizing interaction with fibers. The neutralization of the 5 spinning finishing agent in these two steps, with the associated pH measurements, results in a balance between the stability of the active components and the skin friendliness of the product. Through this methodical approach of separate pH measurements after every base addition, a controlled and stable environment is created that is crucial for the performance of the spin finisher. This allows the benefits of the product, such as the prevention of NOx fading and yellowing, to be optimally utilized.This design offers a robust method to ensure the quality effectiveness of the spin finishing agent, which leads to improved fiber qualities and a longer shelf life of the treated fibers. In a preferred design, the process involves detecting temperature in the reaction vessel using a temperature sensor. The process includes detecting temperature within the reaction vessel to improve the stability of the spin finishing agent formulation. This design optionally includes the use of temperature sensors strategically positioned to monitor and control thermally induced pH fluctuations. Preferably, these sensors are calibrated to detect small changes in temperature, enabling precise adjustments to maintain a stable environment within the reaction vessel. Preferably, the temperature within the reaction vessel is kept within a specific range to prevent rapid evaporation of the first base, which can lead to undesirable temperature increases.The temperature is preferably between 20°C, 30 and 80°C, more preferably between 30°C and 70°C, more preferably between 35°C and 65°C, more preferably between 40°C and 60°C, and most of all between 45°C and 55°C. By maintaining the temperature within these ranges, the reactive environment remains consistent, ensuring reliable quality of the final spin finish.35 Optionally, the temperature control system can include automated feedback mechanisms that adjust heating or cooling elements in response to the data received from the sensors. This system preferably ensures that any deviation from the desired temperature range is quickly corrected, thereby minimizing the risk of pH instability. In this way, temperature control contributes to a more predictable reaction process, which is essential for producing a spin finish with consistent properties.Moreover, precise temperature control in the reaction vessel can be linked to preventing excessive evaporation of volatile components, particularly the first base. This control is preferably achieved through the integration of advanced sensor technology and responsive control systems, which together create a stable and controlled reaction environment. This stability is crucial for achieving the desired chemical interactions and maintaining the integrity of the spin-finishing agent, which ultimately leads to improved performance and durability of the treated fibers. In this preferred implementation, careful management of temperature fluctuations is a key factor in the successful production of a high-quality spin-finishing agent. In a preferred implementation, the method involves the combination of two different bases for accurate and stable pH control, which contributes to the improvement of the overall quality and effectiveness of the spin-finishing agent.This combination offers long-term protection of fibers through controlled acidification after evaporation, which prevents oxidative degradation. This significantly improves fiber quality and durability. 25 Preferably, a volatile base, such as ammonia, is used in the first step of the procedure to lower the pH to an intermediate level. This intermediate pH level can vary, but is preferably between 4.5 and 5.5, more preferably between 4.8 and 5.2, and most preferably at 5. This step is crucial because it enables an initial stabilization of the chemical composition of the spin finishing agent.30 In the next step, a non-volatile base, such as triethanolamine, is added to further raise the pH to a neutral level. This neutral epH level can preferably lie between 6.8 and 8.2, more preferably between 7.0 and 7.8, even more preferably between 7.2 and 7.6, and most preferably at 7.4.This carefully controlled pH increase ensures an optimal balance35 between the stability of the active components and the skin friendliness of the spin finishing agent during use. Optionally, the combination of the two bases ensures that only soluble salts are formed, which further promotes the chemical stability 2024 / 5966 BE2024 / 5966 13 of the product. These soluble salts contribute to the consistency of the pH control and prevent the formation of insoluble salts that could impair the action of the spin finishing agent. Moreover, the controlled acidification that occurs after evaporation of the water can improve the effectiveness of the agent against microbial contamination. This aspect makes the spin finishing agent particularly suitable for applications where increased microbial resistance is desired, such as in humid or warm environments. The acidification also contributes to better adhesion of the agent to the fibers, resulting in improved fiber quality and durability.10 In a preferred design, the method involves stirring and mixing in the reaction vessel using a stirring device, and that the stirring device comprises at least one stirring element on a stirring shaft. This stirring device is preferably designed to ensure uniform mixing of the components,15 which contributes to the consistency of the pH level and the stability of the spin finishing agent. Uniform stirring and mixing preferably reduces the risk of base-induced hydrolysis and associated side reactions of certain organic components. This results in a consistent distribution of the spin finishing agent within the fibers, which can lead to improved20 product quality. The stirring system can optionally contain various types of stirring elements, such as paddles, blades, or impellers, which are designed to improve mixing efficiency. Preferably, the stirring speed can be adjusted to optimize the mixing process, so that all components are evenly distributed throughout the reaction vessel.This uniform mixing is particularly desirable because it ensures a more homogeneous product, which is crucial for maintaining the desired properties of the spin finishing agent. 30 In a more preferred configuration, the stirring system operates at a speed that ensures the minimization of shear forces that could potentially break sensitive components. This consideration is particularly important when dealing with delicate organic compounds that are susceptible to degradation under high shear conditions. By maintaining a controlled stirring speed,35 the integrity of these components is preserved, which further improves the stability and effectiveness of the spin finishing agent. 2024 / 5966 BE2024 / 5966 14 Moreover, the stirring system can also be equipped with temperature control functions, which are optionally designed to keep the reaction vessel at an optimal temperature range.This temperature control is preferably between 20°C and 80°C, more preferably between 25°C and 75°C, even more preferably between 30°C and 70°C, even more preferably between 35°C and 65°C, and most preferably between 40°C and 60°C. Maintaining the reaction within this temperature range is beneficial because it ensures that the reaction kinetics are favorable, thereby promoting the desired chemical interactions without causing thermal degradation of the components. In general, in this preferred design, the integration of a stirring unit with at least one stirring element is a crucial aspect of the process, which offers improved control over the mixing and reaction conditions, which in turn contributes to the production of a high-quality spin finishing agent. 15 In a preferred configuration, pumping and mixing in the reaction vessel will be carried out using an external pump. This pump ensures an even distribution of all components. This preferred configuration contributes to consistent product quality and increases efficiency in subsequent processes.The external pump evenly distributes the first and second bases, which prevents the formation of high local concentrations that could otherwise cause component degradation. This leads to a uniform distribution of the spin finishing agent in the fibers, resulting in improved product quality. Preferably, the external pump can have a capacity ranging between 50 and 200 liters per minute, more preferably between 75 and 175 liters per minute, more preferably between 100 and 150 liters per minute, and most preferably between 120 and 130 liters per minute. This capacity ensures that the components are mixed optimally and evenly, which further promotes the homogeneity of the spin finishing agent. Furthermore, the external pump can preferably be made of stainless steel or another corrosion-resistant material, which benefits the durability and reliability of the system.In an even more preferred configuration, the pump can be equipped with variable speed control, giving the user the ability to adapt the pump operation to specific process requirements. 2024 / 5966 BE2024 / 5966 15 Furthermore, in a preferred configuration, the external pump can be integrated with an automated control system that continuously monitors the pH value and temperature of the mixture. This system can preferably adjust the pump operation based on real-time data, ensuring optimal process control and consistency in the final quality of the spin finishing agent. By combining these preferred features, the use of an external pump in this context offers significant advantages in terms of product quality, process efficiency, and operational reliability. Thisco.