Preparation method of regenerated colored polyester fiber

Abstract

The invention discloses a preparation method of a regenerated colored polyester fiber, the regenerated colored polyester comprises regenerated polyester and pigment, the preparation method comprises the following steps: melting the regenerated colored polyester to obtain a regenerated colored polyester melt, the regenerated colored polyester fiber is prepared from the regenerated colored polyester melt through metering, spinneret plate extrusion, cooling, oiling, stretching, heat setting and winding, and an oil agent adopted in the oiling step at least comprises mineral oil and iso-tridecanol polyoxyethylene ether. According to the invention, the static friction coefficient mu s and the dynamic friction coefficient mu d are adjusted through the oil agent to obtain the cohesive force suitable for the fiber, so that the wear resistance of the fiber is improved, broken filaments generated by breakage of the fiber in the spinning process are reduced, and the machinability of the fiber is improved.

Description

Technical Field

[0001] The invention relates to the technical field of spinning production, and in particular to a method for preparing regenerated colored polyester fibers. Background Art

[0002] Polyethylene terephthalate (PET) has an excellent cost-effectiveness and has been developed and promoted very rapidly. It is currently the dominant material used in the field of chemical fiber and food packaging. As a petroleum-based synthetic polymer material that is not easily degraded, the social reserves of its waste products are also very huge. In view of the pressure from environmental protection and resources, the research on the recycling of PET is becoming a hot topic of concern.

[0003] With the dramatic increase in global polyester production capacity, PET, as an important component of white solid pollutants, has brought increasing pressure to the environment. PET solid waste mostly comes from bottle flakes, diaphragms, films, clothing and non-woven fabrics, as well as waste yarn, waste blocks, powder, etc. generated in various processes of polyester and fiber production. With the increasing depletion of oil resources and increasing environmental pressure, especially the rapid expansion of China's chemical fiber production capacity, the amount of waste yarn generated in the field of polyester industrial yarn has become even more serious.

[0004] There are two methods for recycling PET: physical and chemical. Although chemical recycling can produce relatively pure polymers, there are not many companies that have truly industrialized it. So far, only a few companies have successfully applied it. At this stage, physical methods are still the main method. For recycled fibers, due to different sources of raw materials, there will inevitably be differences in color, purity, viscosity, additives, etc., and they will inevitably contain impurities of different components. In other words, the performance of the raw materials varies greatly, so they are mainly used to produce low-grade staple fibers.

[0005] In the production of recycled colored yarn, small single-filament tripping often occurs. Tripping refers to the occurrence of part of the yarn deviating from the normal winding trajectory and changing from an arc to a string, with a length exceeding 3cm. The occurrence of tripping seriously affects the unwinding performance of the winding bobbin, causing broken ends and hairy yarns in post-processing.

[0006] How to improve the quality of recycled fiber will be of great practical significance. As we all know, chemical recycling is the only method of recycling waste polyester that can achieve closed-loop and sustainable development. Compared with physical recycling, it has high energy consumption, complex technology and greater impact on the environment. There are certain industrial applications in this regard abroad, and physical recycling will still be the mainstream in my country in the next 5 to 10 years. At present, the recycling of polyester in my country mainly uses recycled polyester bottle recycled fibers. These fibers are also mainly some low-end cotton and filling products. Due to the expansion of production capacity and serious homogeneity, recycled fibers are also in a state of micro-profit. Therefore, the high-end and differentiated regenerated fibers are very necessary. It is in this context that we have established a project to produce 100,000 tons of recycled polyester filaments per year using polyester bottle flakes, in order to provide a feasible route for the recycling of high-end polyester products. Therefore, a new technical solution is urgently needed to solve at least one of the above technical problems. Summary of the invention

[0007] In view of the above-mentioned deficiencies, the object of the present invention is to provide a method for preparing regenerated colored polyester fibers, by adjusting the static friction coefficient μs and the dynamic friction coefficient μd by an oil agent to obtain a suitable cohesive force of the fibers, increase the wear resistance of the fibers, prevent the occurrence of thread snags, reduce the amount of lint caused by fiber breakage during the spinning process, and improve the processability of the fibers.

[0008] In order to achieve the above technical objectives and meet the above technical requirements, the technical solution adopted by the present invention is:

[0009] A method for preparing regenerated colored polyester fiber, characterized in that the regenerated colored polyester includes regenerated polyester and pigment, and the preparation method includes the following steps: the regenerated colored polyester is melted to obtain a regenerated colored polyester melt, and the regenerated colored polyester melt is subjected to metering, spinneret extrusion, cooling, oiling, stretching, networking, and winding to obtain the regenerated colored polyester fiber, and the oil agent used in the oiling step includes at least mineral oil and isomeric tridecanol polyoxyethylene ether.

[0010] As a preferred technical solution, the content of the pigment is 0.8-1.2 wt%.

[0011] As a preferred technical solution, the intrinsic viscosity of the recycled colored polyester melt is 0.615-0.630 dL / g.

[0012] As a preferred technical solution, the oil agent includes 10-20 parts of mineral oil, 30-40 parts of polyethylene glycol oleate, 20-30 parts of pentaerythritol oleate, 40-50 parts of isomeric tridecanol polyoxyethylene ether, 10-15 parts of amino silicone oil, 5-8 parts of potassium phosphate, 2-7 parts of sodium alkyl sulfonate, and 1-5 parts of triethanolamine sulfate of fatty alcohol polyoxyethylene ether. The potassium phosphate is potassium phosphate of isomeric tridecanol polyoxyethylene ether or potassium phosphate of dodecanol, and the sodium alkyl sulfonate is sodium dodecyl sulfonate, sodium pentadecyl sulfonate or sodium hexadecyl sulfonate.

[0013] As a preferred technical solution, the steps for preparing the oil agent are as follows: uniformly mix polyethylene glycol oleate, pentaerythritol oleate, isomeric tridecanol polyoxyethylene ether, amino silicone oil, potassium phosphate and sodium alkyl sulfonate, then add mineral oil, stir evenly to obtain the oil agent, the stirring temperature is 40-55°C, and the time is 1-3h.

[0014] As a preferred technical solution, the steps for preparing the amino silicone oil are as follows: hydrogen-containing silicone oil, catalyst chloroplatinic acid, and toluene are added into a reaction container, and acrylamine is added dropwise under stirring, wherein the molar ratio of acrylamine to the hydrogen content in the hydrogen-containing silicone oil is 1.0:(1.0-1.1), the mass ratio of toluene to the hydrogen-containing silicone oil is 1.0:(0.8-0.9), the amount of catalyst chloroplatinic acid used is 0.02% of the mass of the hydrogen-containing silicone oil, the acrylamine titration time is 1.5-2h, the reaction temperature is 60-80°C, after reacting for 1-1.5h, excess n-propanol is added within 30min, stirred evenly, and the product is subjected to reduced pressure distillation to remove the solvent and the remaining acrylamine and n-propanol to obtain the amino silicone oil.

[0015] As a preferred technical solution, the hydrogen-containing silicone oil includes double-end hydrogen-containing silicone oil and end-side hydrogen-containing silicone oil, and the mass ratio of the double-end hydrogen-containing silicone oil to the end-side hydrogen-containing silicone oil is 1:(0.6-0.8).

[0016] As a preferred technical solution, the viscosity of the double-terminal hydrogen-containing silicone oil is 50-100 mPa·s, and the structural formula of the double-terminal hydrogen-containing silicone oil is:

[0017]

[0018] Wherein, x is a positive integer from 3 to 120;

[0019] The viscosity of the end-side hydrogenated silicone oil is 50-100 mPa·s, and the structural formula of the end-side hydrogenated silicone oil is:

[0020]

[0021] Wherein, y and z are positive integers, and the sum of y and z is 10-30;

[0022] As a preferred technical solution, the thermal weight loss of the oil agent after heating at 200°C for 2h is less than 15wt%, the surface tension of the oil agent is 28.2-29.6mN / m, the static friction coefficient between fibers is 0.288-0.296, and the dynamic friction coefficient is 0.274-0.283.

[0023] As a preferred technical solution, the specific parameters of the preparation method are as follows: spinning temperature is 280-290°C, cooling temperature is 20-25°C, network pressure is 0.20-0.30MPa, one roller speed is 2200-2400m / min, one roller temperature is 80-85°C, second roller speed is 3800-4000m / min, second roller temperature is 135-155°C, winding speed is 3750-3940m / min;

[0024] The regenerated colored polyester fiber has a fineness of 75-150 dtex, a breaking strength of ≥3.8 cN / dtex, an elongation at break of 45.0±5.0%, a linear density deviation rate of ≤1.0%, a breaking strength CV value of ≤5.0%, a breaking elongation CV value of ≤8.0%, and a network degree of 13±3 pieces / m.

[0025] Compared with the traditional technical solution, the beneficial effects of the present invention are:

[0026] 1) By adjusting the static friction coefficient μs and the dynamic friction coefficient μd through oil, the fiber can obtain a suitable cohesive force, increase the wear resistance of the fiber, prevent the occurrence of tripping, reduce the fiber breakage during the spinning process and produce hair, and improve the processability of the fiber;

[0027] 2) Mineral oil is cheap, has good smoothness at low temperature, and has good oiling performance. Polyethylene glycol oleate and pentaerythritol oleate have good smoothness, good heat resistance and wear resistance, but polyethylene glycol oleate and pentaerythritol oleate have weak bundling of filaments. The bundling of fibers is adjusted by adding mineral oil. Therefore, on the basis of solving the problem of fiber smoothness and partial bundling, isomeric tridecyl alcohol polyoxyethylene ether is introduced. Isomeric tridecyl alcohol polyoxyethylene ether is a nonionic surfactant with high surface activity and excellent wetting performance, which ensures that the oil can be evenly attached to the silk very quickly during high-speed spinning, so that the oil has good wettability, which is beneficial to improving the smoothness of the oil, and has good wettability, spreadability and permeability.

[0028] 3) Introducing amino substituents into the molecular structure of silicone oil can increase the polarity of silicone oil molecules, produce strong directional adsorption with fibers, and interact with carboxyl, hydroxyl, etc. in fiber macromolecules to form strong directional adsorption. The compounding of double-ended hydrogen-containing silicone oil and end-side hydrogen-containing silicone oil can improve the strength of the oil film, which is beneficial to increase the wear resistance of the fiber. DETAILED DESCRIPTION

[0029] The present invention is further described below.

[0031] An embodiment of the present invention provides a method for preparing a regenerated colored polyester fiber, wherein the regenerated colored polyester includes a regenerated polyester and a pigment, and the preparation method includes the following steps: the regenerated colored polyester is melted to obtain a regenerated colored polyester melt, and the regenerated colored polyester melt is subjected to metering, spinneret extrusion, cooling, oiling, stretching, networking, and winding to obtain the regenerated colored polyester fiber, and the oil agent used in the oiling step includes at least mineral oil and isotridecyl alcohol polyoxyethylene ether.

[0032] The specific parameters of the preparation method are as follows: the spinning temperature is 280-290°C, the cooling temperature is 20-25°C, the network pressure is 0.20-0.30MPa, the speed of the first roller is 2200-2400m / min, the temperature of the first roller is 80-85°C, the speed of the second roller is 3800-4000m / min, the temperature of the second roller is 135-155°C, the winding speed is 3750-3940m / min, stretching is performed between the first roller and the second roller, the second roller is used for heat setting, and the spinning temperature is the extrusion temperature of the spinneret.

[0033] The inventor aims to establish a recycled polyester filament production line with an annual output of 100,000 tons using waste polyester bottle flakes. The inventor conducts a comprehensive analysis of the feasibility of the project, the process route, etc., and finally proposes a specific technical solution. The inventor uses oil to adjust the static friction coefficient μs and the dynamic friction coefficient μd to obtain a suitable cohesive force for the fiber, increase the wear resistance of the fiber, prevent the occurrence of thread tripping, reduce the fuzz caused by fiber breakage during the spinning process, and improve the processability of the fiber.

[0034] In some embodiments, the content of the pigment is 0.8-1.2 wt %. When the content of the pigment is lower than 0.8 wt %, the color is light, and when the content of the pigment is lower than 1.2 wt %, the color is dark, generally black or red.

[0035] In some embodiments, the recycled polyester is recycled polyester from bottle flakes, waste silk or foam materials, and the intrinsic viscosity of the recycled colored polyester melt is 0.615-0.630 dL / g. When the intrinsic viscosity of the recycled colored polyester melt is less than 0.615 or greater than 0.630, the recycled colored polyester fiber is easy to form.

[0036] In some embodiments, the oil agent includes 10-20 parts of mineral oil, 30-40 parts of polyethylene glycol oleate, 20-30 parts of pentaerythritol oleate, 40-50 parts of isomeric tridecanol polyoxyethylene ether, 10-15 parts of amino silicone oil, 5-8 parts of potassium phosphate, 2-7 parts of sodium alkyl sulfonate, and 1-5 parts of triethanolamine sulfate of fatty alcohol polyoxyethylene ether. The potassium phosphate is potassium phosphate of isomeric tridecanol polyoxyethylene ether or potassium phosphate of dodecanol, and the sodium alkyl sulfonate is sodium dodecyl sulfonate, sodium pentadecyl sulfonate or sodium hexadecyl sulfonate.

[0037] The steps of preparing the oil are as follows: uniformly mix polyethylene glycol oleate, pentaerythritol oleate, isomeric tridecanol polyoxyethylene ether, amino silicone oil, potassium phosphate and sodium alkyl sulfonate, then add mineral oil, stir evenly to obtain the oil, and the mixing is carried out at room temperature, that is, the stirring temperature is 40-55°C, and the stirring time is 1-3h.

[0038] The reasons for the occurrence of wire tripping include equipment, process, melt quality, etc. After the problems of equipment and melt quality are solved, an important factor causing wire tripping is the oil problem in the process. Increasing or decreasing the oil content will slightly improve the wire tripping, but it is not solved; the oil content has a great influence on the winding formation. If the amount of oil is too much, the silk layer will slip and the end surface of the silk cake will be uneven; if the oil is too little, the silk cake will be tightly wound, unwinding will be difficult, and the silk cake will be very stiff. In addition, increasing the number of network points, the winding tension will decrease, and the wire tripping situation will become worse; reducing the number of network points, the winding tension will increase, and the wire tripping will be slightly improved, but too few network points will not meet the product requirements and will increase the physical property degradation of the silk cake caused by the small number of network points. While ensuring that the oil concentration and oil content are close, there is no obvious improvement in the yarn tripping problem when changing different oils. This is because for colored yarns, the dynamic friction coefficient between the fibers involved in the existing oils is mostly between 0.26-0.27, and the static friction coefficient is between 0.19-0.20. The static friction coefficient is too low, indicating that its bundling is weak.

[0039] The definition of cohesion is the attraction between fibers, which is related to fiber properties such as fiber surface, friction, fiber cross-sectional shape and linear density. Fibers with smooth surfaces produce greater cohesion than fibers with rough surfaces. When the cohesion decreases, the fiber bundle becomes loose, causing friction between the fiber and the yarn guide assembly, that is, the friction between the fiber and the ceramic increases, which is the main reason for the damage of the yarn. Compared with white yarn, colored yarn has a higher impurity content and a smaller friction contact area between fibers, so the friction coefficient decreases accordingly, resulting in a decrease in the cohesion of the fiber. The lower friction coefficient leads to a decrease in the cohesion performance between the single yarns and the occurrence of tripping yarns.

[0040] The cohesion is adjusted by oil. The performance change trend of the main components of the oil from mineral oil, fatty alcohol, polyol ester to polyether is that the bundle of the filaments changes from good to poor, and the film strength changes from poor to strong. Mineral oil is widely used in chemical fiber spinning oils because it is cheap, has good smoothness at low temperatures, and has good oiling performance. Oleic acid polyethylene glycol ester and pentaerythritol oleate have good smoothness, moderate heat resistance and wear resistance. However, oleic acid polyethylene glycol ester and pentaerythritol oleate have weak bundle of filaments, which is difficult to meet the demand for the cohesion of colored silk fibers. The problem of fiber smoothness and partial bundle is solved by compounding oleic acid polyethylene glycol ester and pentaerythritol oleate with mineral oil.

[0041] Therefore, on the basis of solving the problem of fiber smoothness and partial bundling, isomeric tridecanol polyoxyethylene ether is introduced. Isomeric tridecanol polyoxyethylene ether is a nonionic surfactant, which has high surface activity and excellent wetting properties. The performance of the wetting agent determines the wetting, spreading, penetration and diffusion speed of the oil agent on the fiber surface, ensuring that the oil agent can be evenly attached to the silk very quickly during high-speed spinning. Isomeric tridecanol polyoxyethylene ether shows excellent emulsifying power, which is that the interfacial film formed by the branching of the hydrophobic group is stronger, and the emulsion formed is more stable. At the same time, its HLB value is small, that is, the hydrophilic-lipophilic balance value, so that the oil agent has good wettability. Isomeric tridecanol polyoxyethylene ether has high stability and compatibility in aqueous solution, which is conducive to improving the smoothness of the oil agent and has good wettability, spreading and permeability.

[0042] In some embodiments, the steps of preparing the amino silicone oil are as follows: hydrogen-containing silicone oil, catalyst chloroplatinic acid, and toluene are added to a reaction vessel, and acrylamine is added dropwise under stirring, wherein the molar ratio of acrylamine to the hydrogen content in the hydrogen-containing silicone oil is 1.0:(1.0-1.1), the mass ratio of toluene to the hydrogen-containing silicone oil is 1.0:(0.8-0.9), and the amount of catalyst chloroplatinic acid is 0.02% of the mass of the hydrogen-containing silicone oil. The acrylamine titration time is 1.5-2h, the reaction temperature is 60-80°C, after reacting for 1-1.5h, excess n-propanol is added within 30min, stirred evenly, and the product is subjected to reduced pressure distillation to remove the solvent and the remaining acrylamine and n-propanol to obtain amino silicone oil.

[0043] In some embodiments, the hydrogen-containing silicone oil includes double-end hydrogen-containing silicone oil and end-side hydrogen-containing silicone oil, and the mass ratio of the double-end hydrogen-containing silicone oil to the end-side hydrogen-containing silicone oil is 1:(0.6-0.8).

[0044] In some embodiments, the viscosity of the double-terminal hydrogen-containing silicone oil is 50-100 mPa·s, and the structural formula of the double-terminal hydrogen-containing silicone oil is:

[0045]

[0046] Wherein, x is a positive integer from 3 to 120;

[0047] The viscosity of the end-side hydrogenated silicone oil is 50-100 mPa·s, and the structural formula of the end-side hydrogenated silicone oil is:

[0048]

[0049] Wherein, y and z are positive integers, and the sum of y and z is 10-30;

[0050] Introducing amino substituents into the molecular structure of silicone oil can increase the polarity of silicone oil molecules, produce strong directional adsorption with fibers, and interact with carboxyl, hydroxyl, etc. in fiber macromolecules to form strong directional adsorption. The compounding of double-ended hydrogen-containing silicone oil and end-side hydrogen-containing silicone oil can improve the strength of the oil film, which is beneficial to increase the wear resistance of the fiber, reduce the hair caused by fiber breakage during the spinning process, and improve the processability of the fiber.

[0051] The size of the static friction coefficient has a great influence on the cohesion and smoothness. Colored silk oil requires both to be excellent and suitable. To obtain good cohesion, the static friction coefficient μs of the fiber should be large.

[0052] The present invention selects isomeric tridecanol polyoxyethylene ether, mineral oil, oleic acid polyethylene glycol ester and pentaerythritol oleate, and more importantly, obtains suitable fiber cohesion by adjusting the static friction coefficient μs and the dynamic friction coefficient μd. The static friction coefficient between the fibers of the present invention is 0.230-0.246, the dynamic friction coefficient is 0.274-0.283, the difference between the static friction coefficient μs and the dynamic friction coefficient μd is appropriate, and the fiber is smooth and has excellent cohesion.

[0053] Fatty alcohol polyoxyethylene ether triethanolamine sulfate is used as a sizing agent to improve the bundling of fibers. It has good adhesion and permeability to fibers, but its own viscosity is high, which will cause the viscosity of the oil to be too high. A small amount is added to adjust the cohesion of the fibers.

[0054] In some embodiments, the thermal weight loss of the oil agent after heating at 200° C. for 2 hours is less than 15wt%, the surface tension of the oil agent is 28.2-29.6mN / m, the static friction coefficient between the fibers is 0.288-0.296, and the dynamic friction coefficient is 0.274-0.283.

[0055] The regenerated colored polyester fiber has a fineness of 75-150 dtex, a breaking strength of ≥3.8 cN / dtex, an elongation at break of 45.0±5.0%, a linear density deviation rate of ≤1.0%, a breaking strength CV value of ≤5.0%, a breaking elongation CV value of ≤8.0%, and a network degree of 13±3 pieces / m.

[0056] Example 1

[0057] A method for preparing regenerated colored polyester fiber, wherein the regenerated colored polyester comprises regenerated polyester and a pigment, and the preparation method comprises the following steps: the regenerated colored polyester is melted to obtain a regenerated colored polyester melt, and the regenerated colored polyester melt is metered, extruded from a spinneret, cooled, oiled, stretched, networked, and wound to obtain the regenerated colored polyester fiber, wherein the oil agent used in the oiling step comprises at least mineral oil and isomeric tridecanol polyoxyethylene ether, the content of the pigment is 0.8wt%, and the characteristic viscosity of the regenerated colored polyester melt is 0.615dL / g.

[0058] The specific parameters of the preparation method are as follows: spinning temperature is 280°C, cooling temperature is 20°C, network pressure is 0.20MPa, first roller speed is 2200m / min, first roller temperature is 80°C, second roller speed is 3800m / min, second roller temperature is 135°C, winding speed is 3750m / min, and stretching is performed between the first roller and the second roller.

[0059] The oil agent includes 10 parts of mineral oil, 30 parts of polyethylene glycol oleate, 20 parts of pentaerythritol oleate, 40 parts of isomeric tridecanol polyoxyethylene ether, 10 parts of amino silicone oil, 5 parts of potassium phosphate, 2 parts of sodium alkyl sulfonate, 1 part of triethanolamine sulfate of fatty alcohol polyoxyethylene ether, the potassium phosphate is potassium phosphate of isomeric tridecanol polyoxyethylene ether, and the sodium alkyl sulfonate is sodium dodecyl sulfonate.

[0060] The steps of preparing the oil are as follows: uniformly mix polyethylene glycol oleate, pentaerythritol oleate, isomeric tridecanol polyoxyethylene ether, amino silicone oil, potassium phosphate and sodium alkyl sulfonate, add mineral oil, and stir to obtain the oil. The stirring temperature is 40° C. and the time is 1 hour.

[0061] The steps for preparing amino silicone oil are as follows: hydrogen-containing silicone oil, catalyst chloroplatinic acid and toluene are added into a reaction container, and acrylamine is added dropwise under stirring, wherein the molar ratio of acrylamine to the hydrogen content in the hydrogen-containing silicone oil is 1.0:1.0, the mass ratio of toluene to the hydrogen-containing silicone oil is 1.0:0.8, the amount of catalyst chloroplatinic acid used is 0.02% of the mass of the hydrogen-containing silicone oil, the acrylamine titration time is 1.5h, the reaction temperature is 60°C, after reacting for 1h, excess n-propanol is added within 30min, stirred evenly, and the product is subjected to reduced pressure distillation to remove the solvent and the remaining acrylamine and n-propanol to obtain amino silicone oil.

[0062] The hydrogen-containing silicone oil includes double-end hydrogen-containing silicone oil and end-side hydrogen-containing silicone oil, and the mass ratio of the double-end hydrogen-containing silicone oil to the end-side hydrogen-containing silicone oil is 1:0.6.

[0063] The viscosity of the double-ended hydrogen-containing silicone oil is 50mPa·s, and the structural formula of the double-ended hydrogen-containing silicone oil is:

[0064]

[0065] Where x is 3;

[0066] The viscosity of the end-side hydrogen-containing silicone oil is 50mPa·s, and the structural formula of the end-side hydrogen-containing silicone oil is:

[0067]

[0068] In the formula, y and z are positive integers, y is 10, z is 20;

[0069] The oil agent loses 13.3 wt % of its weight after being heated at 200° C. for 2 h. The surface tension of the oil agent is 28.2 mN / m. The static friction coefficient between the fibers is 0.288, and the dynamic friction coefficient is 0.274.

[0070] The fineness of the recycled colored polyester fiber is 75 dtex, the breaking strength is 3.93 cN / dtex, the breaking elongation is 47.2%, the linear density deviation rate is 0.88%, the breaking strength CV value is 4.2%, the breaking elongation CV value is 6.2%, and the network degree is 15 pieces / m.

[0071] Example 2

[0072] A method for preparing regenerated colored polyester fiber, wherein the regenerated colored polyester comprises regenerated polyester and a pigment, and the preparation method comprises the following steps: the regenerated colored polyester is melted to obtain a regenerated colored polyester melt, and the regenerated colored polyester melt is metered, extruded from a spinneret, cooled, oiled, stretched, networked, and wound to obtain the regenerated colored polyester fiber, wherein the oil agent used in the oiling step comprises at least mineral oil and isomeric tridecanol polyoxyethylene ether, the content of the pigment is 1wt%, and the characteristic viscosity of the regenerated colored polyester melt is 0.62dL / g.

[0073] The specific parameters of the preparation method are as follows: spinning temperature is 285°C, cooling temperature is 23°C, network pressure is 0.25MPa, first roller speed is 2300m / min, first roller temperature is 83°C, second roller speed is 3900m / min, second roller temperature is 140°C, winding speed is 3800m / min, and stretching is performed between the first roller and the second roller.

[0074] The oil agent includes 15 parts of mineral oil, 35 parts of polyethylene glycol oleate, 25 parts of pentaerythritol oleate, 45 parts of isomeric tridecanol polyoxyethylene ether, 12 parts of amino silicone oil, 6 parts of potassium phosphate, 5 parts of sodium alkyl sulfonate, 3 parts of triethanolamine sulfate of fatty alcohol polyoxyethylene ether, the potassium phosphate is potassium phosphate of isomeric tridecanol polyoxyethylene ether, and the sodium alkyl sulfonate is sodium pentadecyl sulfonate.

[0075] The steps of preparing the oil are as follows: uniformly mix polyethylene glycol oleate, pentaerythritol oleate, isomeric tridecanol polyoxyethylene ether, amino silicone oil, potassium phosphate and sodium alkyl sulfonate, add mineral oil, and stir uniformly to obtain the oil. The stirring temperature is 50° C. and the time is 2 hours.

[0076] The steps of preparing amino silicone oil are as follows: hydrogen-containing silicone oil, catalyst chloroplatinic acid, and toluene are added into a reaction vessel, and acrylamine is added dropwise under stirring, wherein the molar ratio of acrylamine to the hydrogen content in the hydrogen-containing silicone oil is 1.0:1.0, the mass ratio of toluene to the hydrogen-containing silicone oil is 1.0:0.8, and the amount of catalyst chloroplatinic acid is 0.02% of the mass of the hydrogen-containing silicone oil. The acrylamine titration time is 1.5 hours, the reaction temperature is 70°C, after reacting for 1.2 hours, excess n-propanol is added within 30 minutes, stirred evenly, and the product is subjected to reduced pressure distillation to remove the solvent and the remaining acrylamine and n-propanol to obtain amino silicone oil.

[0077] The hydrogen-containing silicone oil includes double-end hydrogen-containing silicone oil and end-side hydrogen-containing silicone oil, and the mass ratio of the double-end hydrogen-containing silicone oil to the end-side hydrogen-containing silicone oil is 1:0.7.

[0078] The viscosity of the double-ended hydrogen-containing silicone oil is 70mPa·s, and the structural formula of the double-ended hydrogen-containing silicone oil is:

[0079]

[0080] Wherein, x is 68;

[0081] The viscosity of the end-side hydrogenated silicone oil is 80 mPa·s, and the structural formula of the end-side hydrogenated silicone oil is:

[0082]

[0083] Where yy is 20, z is 10;

[0084] The oil agent loses 14.2 wt % of its weight after being heated at 200° C. for 2 h. The surface tension of the oil agent is 29 mN / m. The static friction coefficient between the fibers is 0.292, and the dynamic friction coefficient is 0.280.

[0085] The fineness of the recycled colored polyester fiber is 100 dtex, the breaking strength is 3.96 cN / dtex, the breaking elongation is 45.6%, the linear density deviation rate is 1.0%, the breaking strength CV value is 4.8%, the breaking elongation CV value is 6.3%, and the network degree is 13 pieces / m.

[0086] Example 3

[0087] A method for preparing regenerated colored polyester fiber, wherein the regenerated colored polyester comprises regenerated polyester and a pigment, and the preparation method comprises the following steps: the regenerated colored polyester is melted to obtain a regenerated colored polyester melt, and the regenerated colored polyester melt is subjected to metering, spinneret extrusion, cooling, oiling, stretching, networking, and winding to obtain the regenerated colored polyester fiber, wherein the oiling agent used in the oiling step comprises at least mineral oil and isomeric tridecanol polyoxyethylene ether, the content of the pigment is 1.2wt%, and the characteristic viscosity of the regenerated colored polyester melt is 0.630dL / g.

[0088] The specific parameters of the preparation method are as follows: spinning temperature is 290°C, cooling temperature is 25°C, network pressure is 0.30MPa, first roller speed is 2400m / min, first roller temperature is 85°C, second roller speed is 4000m / min, second roller temperature is 155°C, winding speed is 3940m / min, and stretching is performed between the first roller and the second roller.

[0089] The oil agent includes 20 parts of mineral oil, 40 parts of polyethylene glycol oleate, 30 parts of pentaerythritol oleate, 50 parts of isomeric tridecanol polyoxyethylene ether, 15 parts of amino silicone oil, 8 parts of potassium phosphate, 7 parts of sodium alkyl sulfonate, 5 parts of triethanolamine sulfate of fatty alcohol polyoxyethylene ether, the potassium phosphate is potassium tetradecanol phosphate, and the sodium alkyl sulfonate is sodium hexadecyl sulfonate.

[0090] The steps of preparing the oil are as follows: uniformly mix polyethylene glycol oleate, pentaerythritol oleate, isomeric tridecanol polyoxyethylene ether, amino silicone oil, potassium phosphate and sodium alkyl sulfonate, add mineral oil, and stir uniformly to obtain the oil. The stirring temperature is 55° C. and the time is 3 hours.

[0091] The steps of preparing amino silicone oil are as follows: hydrogen-containing silicone oil, catalyst chloroplatinic acid, and toluene are added to a reaction vessel, and acrylamine is added dropwise under stirring, wherein the molar ratio of acrylamine to the hydrogen content in the hydrogen-containing silicone oil is 1.0:1.1, the mass ratio of toluene to the hydrogen-containing silicone oil is 1.0:0.9, and the amount of catalyst chloroplatinic acid is 0.02% of the mass of the hydrogen-containing silicone oil. The acrylamine titration time is 2 hours, the reaction temperature is 80°C, after reacting for 1.5 hours, excess n-propanol is added within 30 minutes, stirred evenly, and the product is subjected to reduced pressure distillation to remove the solvent and the remaining acrylamine and n-propanol to obtain amino silicone oil.

[0092] The hydrogen-containing silicone oil includes double-end hydrogen-containing silicone oil and end-side hydrogen-containing silicone oil, and the mass ratio of the double-end hydrogen-containing silicone oil to the end-side hydrogen-containing silicone oil is 1:0.8.

[0093] The viscosity of double-ended hydrogen-containing silicone oil is 50-100mPa·s, and the structural formula of double-ended hydrogen-containing silicone oil is:

[0094]

[0095] Wherein, x is a positive integer greater than 120;

[0096] The viscosity of the end-side hydrogenated silicone oil is 50-100 mPa·s, and the structural formula of the end-side hydrogenated silicone oil is:

[0097]

[0098] Wherein, y is 15, z is 15;

[0099] The thermal weight loss of the oil after heating at 200°C for 2h was 13.7%, the surface tension of the oil was 29.6mN / m, the static friction coefficient between the fibers was 0.296, and the dynamic friction coefficient was 0.283.

[0100] The fineness of the recycled colored polyester fiber is 150 dtex, the breaking strength is 4.31 cN / dtex, the breaking elongation is 45.6%, the linear density deviation rate is 0.82%, the breaking strength CV value is 4.5%, the breaking elongation CV value is 6.6%, and the network degree is 16 pieces / m.

[0101] The difference between the static friction coefficient μs and the dynamic friction coefficient μd of the regenerated colored polyester fibers of Example 1, Example 2 and Implementation 3 is appropriate, the smoothness and adhesion are relatively excellent, the mechanical properties of the regenerated colored polyester fibers are excellent, and the thread tripping phenomenon will not occur.

[0102] Any numerical value cited herein includes all values ​​of lower and upper values ​​that increase by one unit from the lower limit to the upper limit, and there is at least a two-unit interval between any lower value and any higher value. For example, if the value of the quantity of a component or a process variable (such as temperature, pressure, time, etc.) is stated to be from 1 to 90, preferably from 20 to 80, and more preferably from 30 to 70, the purpose is to illustrate that values ​​such as 15 to 85, 22 to 68, 43 to 51, 30 to 32 are also explicitly listed in the specification. For values ​​less than 1, one unit is appropriately considered to be 0.0001, 0.001, 0.01, 0.1. These are merely examples that are intended to be clearly expressed, and it can be considered that all possible combinations of numerical values ​​listed between the lowest value and the highest value are clearly stated in the specification in a similar manner.

[0103] Unless otherwise indicated, all ranges include the endpoints and all numbers between the endpoints. "About" or "approximately" used with a range applies to both endpoints of the range. Thus, "about 20 to 30" is intended to cover "about 20 to about 30", including at least the specified endpoints.

[0104] All articles and references disclosed, including patent applications and publications, are incorporated herein by reference for all purposes. The term "consisting essentially of..." to describe a combination should include the identified elements, ingredients, parts or steps and other elements, ingredients, parts or steps that do not substantially affect the basic novel characteristics of the combination. The use of the terms "comprising" or "including" to describe a combination of elements, ingredients, parts or steps herein also contemplates embodiments that consist essentially of these elements, ingredients, parts or steps. By using the term "may", it is intended to indicate that any attribute described that "may" include is optional.

[0105] Multiple elements, ingredients, parts or steps can be provided by a single integrated element, ingredient, part or step. Alternatively, a single integrated element, ingredient, part or step can be divided into separate multiple elements, ingredients, parts or steps. The disclosure "one" or "an" used to describe an element, ingredient, part or step is not intended to exclude other elements, ingredients, parts or steps.

[0106] It should be understood that the above description is for illustration and not for limitation. Many embodiments and many applications beyond the examples provided will be apparent to those skilled in the art upon reading the above description. Therefore, the scope of the present teachings should not be determined with reference to the above description, but should be determined with reference to the appended claims and the full scope of equivalents possessed by such claims. For the purpose of comprehensiveness, all articles and references, including disclosures of patent applications and publications, are incorporated herein by reference. The omission of any aspect of the subject matter disclosed herein in the preceding claims is not intended to be a waiver of the subject matter, nor should it be considered that the inventors did not consider the subject matter to be part of the disclosed inventive subject matter.

Claims

1. A method for preparing regenerated colored polyester fiber, characterized in that: The regenerated colored polyester includes regenerated polyester and pigment, and the preparation method includes the following steps: the regenerated colored polyester is melted to obtain a regenerated colored polyester melt, and the regenerated colored polyester melt is metered, extruded from a spinneret, cooled, oiled, stretched, networked, and wound to obtain the regenerated colored polyester fiber, and the oil agent used in the oiling step includes at least mineral oil and isomeric tridecanol polyoxyethylene ether.

2. The method for preparing regenerated colored polyester fiber according to claim 1, characterized in that: The content of the pigment is 0.8-1.2 wt %.

3. The method for preparing regenerated colored polyester fiber according to claim 1, characterized in that: The intrinsic viscosity of the recycled colored polyester melt is 0.615-0.630 dL / g.

4. The method for preparing regenerated colored polyester fiber according to claim 1, characterized in that: The oil agent comprises 10-20 parts of mineral oil, 30-40 parts of polyethylene glycol oleate, 20-30 parts of pentaerythritol oleate, 40-50 parts of isomeric tridecanol polyoxyethylene ether, 10-15 parts of amino silicone oil, 5-8 parts of potassium phosphate, 2-7 parts of sodium alkyl sulfonate, and 1-5 parts of triethanolamine sulfate of fatty alcohol polyoxyethylene ether. The potassium phosphate is potassium phosphate of isomeric tridecanol polyoxyethylene ether or potassium phosphate of dodecanol, and the sodium alkyl sulfonate is sodium dodecyl sulfonate, sodium pentadecyl sulfonate or sodium hexadecyl sulfonate.

5. The method for preparing regenerated colored polyester fiber according to claim 4, characterized in that: The steps of preparing the oil are as follows: uniformly mix polyethylene glycol oleate, pentaerythritol oleate, isomeric tridecanol polyoxyethylene ether, amino silicone oil, potassium phosphate and sodium alkyl sulfonate, add mineral oil, and stir uniformly to obtain the oil. The stirring temperature is 40-55° C. and the time is 1-3 hours.

6. The method for preparing regenerated colored polyester fiber according to claim 5, characterized in that: The steps of preparing the amino silicone oil are as follows: adding hydrogen-containing silicone oil, catalyst chloroplatinic acid and toluene into a reaction container, and dropping acrylamine under stirring, wherein the molar ratio of acrylamine to the hydrogen content in the hydrogen-containing silicone oil is 1.0:(1.0-1.1), the mass ratio of toluene to the hydrogen-containing silicone oil is 1.0:(0.8-0.9), the amount of catalyst chloroplatinic acid used is 0.02% of the mass of the hydrogen-containing silicone oil, the acrylamine titration time is 1.5-2h, the reaction temperature is 60-80°C, after reacting for 1-1.5h, adding excess n-propanol within 30min, stirring evenly, and removing the solvent and the remaining acrylamine and n-propanol from the product by reduced pressure distillation to obtain the amino silicone oil.

7. The method for preparing regenerated colored polyester fiber according to claim 6, characterized in that: The hydrogen-containing silicone oil comprises double-end hydrogen-containing silicone oil and end-side hydrogen-containing silicone oil, and the mass ratio of the double-end hydrogen-containing silicone oil to the end-side hydrogen-containing silicone oil is 1:(0.6-0.8).

8. The method for preparing regenerated colored polyester fiber according to claim 7, characterized in that: The viscosity of the double-terminal hydrogen-containing silicone oil is 50-100 mPa·s, and the structural formula of the double-terminal hydrogen-containing silicone oil is: Wherein, x is a positive integer from 3 to 120; The viscosity of the end-side hydrogenated silicone oil is 50-100 mPa·s, and the structural formula of the end-side hydrogenated silicone oil is: Wherein, yy and z are positive integers, and the sum of y and z is 10-30.

9. The method for preparing regenerated colored polyester fiber according to claim 6, characterized in that: The thermal weight loss of the oil after heating at 200° C. for 2 hours is less than 15wt%, the surface tension of the oil is 28.2-29.6mN / m, the static friction coefficient between fibers is 0.288-0.296, and the dynamic friction coefficient is 0.274-0.

283.

10. The method for preparing regenerated colored polyester fiber according to claim 1, characterized in that: The specific parameters of the preparation method are as follows: spinning temperature is 280-290°C, cooling temperature is 20-25°C, network pressure is 0.20-0.30MPa, first roller speed is 2200-2400m / min, first roller temperature is 80-85°C, second roller speed is 3800-4000m / min, second roller temperature is 135-155°C, winding speed is 3750-3940m / min; The regenerated colored polyester fiber has a fineness of 75-150 dtex, a breaking strength of ≥3.8 cN / dtex, an elongation at break of 45.0±5.0%, a linear density deviation rate of ≤1.0%, a breaking strength CV value of ≤5.0%, a breaking elongation CV value of ≤8.0%, and a network degree of 13±3 pieces / m.

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