Full-dull polyester fiber and preparation method thereof

Abstract

The invention discloses a full-dull polyester fiber, the full-dull polyester fiber contains titanium dioxide, and an oil agent for oiling the full-dull polyester fiber at least comprises iso-tridecanol polyoxyethylene ether. According to the full-dull polyester fiber, the oiling agent containing iso-tridecanol polyoxyethylene ether is adopted, and the cohesive force suitable for the fiber can be obtained by adjusting the static friction coefficient and the dynamic friction coefficient. The invention also aims to disclose a preparation method of the full-dull polyester fiber, which comprises the following steps: preparing the oil agent, metering and extruding the full-dull polyester to obtain a full-dull polyester melt, cooling, oiling with the oil agent, stretching, carrying out heat setting and winding to prepare the full-dull polyester fiber. The intrinsic viscosity of the full-dull polyester melt is 0.615 to 0.630 dL / g. The preparation method disclosed by the invention is good in controllability, the cohesive force of the prepared full-dull polyester fiber is reasonable, the phenomena of broken filaments and floating filaments cannot be generated in production, and the mechanical property of the full-dull polyester fiber is excellent.

Description

Technical Field

[0001] The invention relates to the technical field of spinning production, in particular to a full-dull polyester fiber and a preparation method thereof. Background Art

[0002] With the development of the economy, people pay more and more attention to the visual effect of fabrics in the production of polyester filaments. In order to achieve the effect of imitating cotton fabrics and eliminate the brighter luster of polyester, manufacturers can add a higher content of titanium dioxide to the filaments to produce full-dull fiber to eliminate the aurora effect of the fabric; at the same time, titanium dioxide additives can play a role in UV protection. When ultraviolet rays pass through the fiber containing the matting agent, they will produce certain ultraviolet absorption and reflection, reducing harm to the human body. Therefore, the development of high-value-added full-dull fiber has become a trend.

[0003] However, with the increase of titanium dioxide content, the friction between fibers decreases significantly. This is mainly because titanium dioxide gathers on the fiber surface, resulting in a decrease in the surface area of ​​the fiber. In the mutual friction, the area of ​​friction contact becomes smaller, so the friction coefficient becomes smaller accordingly, which is more obvious in the friction between the filaments. For filament processing, the oiling method of the oil nozzle can effectively improve the bundling of polyester filaments, the uniformity of oiling, and the continuous stability of the oiling rate. The titanium dioxide particles on the fiber surface of the full-dull POY are seriously agglomerated. After the filaments are solidified and formed, they pass through the oil nozzle at a high speed. Due to the decrease in the cohesive force, the titanium dioxide particles on the fiber surface are easily scraped off during the friction between the fiber and the oil nozzle, forming white powder. When there is more white powder, the oil outlet will be blocked, resulting in a decrease in the oiling rate and uneven oiling rate. In the friction process, it is also easy to break the single filaments by friction, forming floating single filaments.

[0004] The spinning speed of polyester POY is generally 2500-3500m / min. At high spinning speed, the filament and the guide assembly will generate large friction and static electricity, causing the spinning tension to increase, resulting in filament damage, affecting the subsequent processing and filament quality. The friction between the fiber and the guide assembly belongs to the friction between the fiber and the ceramic, including the contact parts such as the nozzle, the guide hook and the pre-network device, which is the main reason for the damage of the filament. If the fiber is not well bonded, the fiber bundle will not be tight and resistant to friction, and it will affect the breaking strength. It is easy to cut and produce lint during the spinning process, affecting production and increasing production costs. In addition, the finished silk will also turn white or lint, and the color absorption will be uneven during dyeing, and it is easy to produce color spots, which seriously affects the color fastness of the fabric. The existing semi-dull fiber oil cannot meet the requirements of good bonding performance of full-dull fiber. In the production process, single filament tripping occurs due to poor bonding of single filaments, which affects the quality of the fiber.

[0005] In the prior art, the occurrence of wire tripping is reduced by adjusting the oil concentration and the oil application rate, but the increase in the oil concentration and the oil application rate brings new problems. If the oil application rate is too high, during the DTY processing, the oil is sprayed on the ceramic friction disk, and the excessive oil adhering to the friction disk due to high-speed rotation friction will melt and accumulate due to heat and adhere to the processing surface of the friction disk and the roller, affecting the deformation effect. If the oil concentration is too high, it will have an adverse effect on wettability, diffusion rate, and oil film coverage. Therefore, a new technical solution is urgently needed to solve at least one of the above technical problems. Summary of the invention

[0006] In view of the above-mentioned shortcomings, one object of the present invention is to provide a fully matte polyester fiber, wherein the oil containing isomeric tridecanol polyoxyethylene ether can adjust the static friction coefficient and the dynamic friction coefficient to obtain a suitable cohesion of the fiber. Another object of the present invention is to disclose a method for preparing a fully matte polyester fiber, which has good controllability, and the cohesion of the prepared fully matte polyester fiber is reasonable, and the phenomenon of tripping, hairy and floating silk will not occur during production, and the fully matte polyester fiber has excellent mechanical properties.

[0007] In order to achieve the above technical objectives and meet the above technical requirements, the technical solution adopted by the present invention is:

[0008] A fully matte polyester fiber, the fully matte polyester fiber contains titanium dioxide, and the oiling agent used for oiling the fully matte polyester fiber at least comprises isomeric tridecanol polyoxyethylene ether.

[0009] As a preferred technical solution, the content of titanium dioxide is 2.0-2.2wt%.

[0010] As a preferred technical solution, the oil agent has the following components in parts by weight: 30-40 parts of EO / PO random copolymerized lauryl alcohol polyether, 30-40 parts of mineral oil, 15-20 parts of isomeric tridecyl alcohol polyoxyethylene ether, 8-10 parts of amino silicone oil, and 8-15 parts of fatty alcohol polyoxyethylene ether potassium salt.

[0011] As a preferred technical solution, the isomeric tridecanol polyoxyethylene ether is one of isomeric tridecanol polyoxyethylene ether 1303, 1305, and 1306.

[0012] The present invention also provides a method for preparing a fully matte polyester fiber, comprising the following steps: preparing the oil agent, metering the fully matte polyester, extruding it to obtain a fully matte polyester melt, cooling it, oiling it with the oil agent, pre-networking it, and winding it to prepare the fully matte polyester fiber, wherein the characteristic viscosity of the fully matte polyester melt is 0.615-0.630dL / g.

[0013] As a preferred technical solution, the steps for preparing the oil agent are as follows: prepare amino silicone oil, mix EO / PO random copolymerized lauryl alcohol polyether, isomeric tridecanol polyoxyethylene ether, the amino silicone oil and fatty alcohol polyoxyethylene ether phosphate potassium salt evenly, add them into the mineral oil and stir evenly to obtain the oil agent, and the mixing is carried out at room temperature, 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, a catalyst, 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), the amount of the catalyst is 0.015-0.020% by weight of the hydrogen-containing silicone oil, the acrylamine titration time is 1.5-2h, the reaction temperature in the reaction vessel is 60-80°C, after reacting for 1-1.5h, an excess of n-propanol is added, and the reaction product is stirred for 1-1.5h, and the solvent and the remaining acrylamine and n-propanol are removed from the reaction product by reduced pressure distillation to obtain the amino silicone oil, and the catalyst is chloroplatinic acid.

[0015] As a preferred technical solution, the viscosity of the hydrogen-containing silicone oil is 50-100 mPa·s, and the structural formula of the hydrogen-containing silicone oil is:

[0016]

[0017] Wherein, x is a positive integer from 3 to 120.

[0018] As a preferred technical solution, the oil film strength of the oil agent is 107-115kg, the surface tension of the oil agent is 31.8-33.2cN / cm, the wetting time is 2.0-2.5s, and after the fully matte polyester fiber is oiled with the oil agent, the static friction coefficient between the fully matte polyester fibers is 0.297-0.305, and the dynamic friction coefficient is 0.286-0.293.

[0019] As a preferred technical solution, the extrusion temperature of the full-dull polyester is 280-290°C, the cooling air temperature of the full-dull polyester is 20-25°C, the pre-network pressure is 0.03±0.005Mpa, and the winding speed of the full-dull polyester is 2500-3000m / min;

[0020] The full-dull polyester fiber has a fineness of 75-150 dtex, a breaking strength of ≥1.8 cN / dtex, a breaking elongation of 120.0±10.0%, a linear density deviation rate of ≤1.2%, a breaking strength CV value of ≤5.0%, a breaking elongation CV value of ≤5.0%, and a yarn evenness CV of ≤1.10%.

[0021] Compared with the traditional technical solution, the beneficial effects of the present invention are:

[0022] 1) The oil containing isomeric tridecanol polyoxyethylene ether can adjust the static friction coefficient and dynamic friction coefficient to obtain the appropriate cohesion of the fiber, solve the problem of poor cohesion due to high content of titanium dioxide, and avoid the problems of filament damage, filament tripping, floating filament and hairy filament;

[0023] 2) EO / PO random copolymerized lauryl alcohol polyether: As EO / PO presents alternating distribution, it can reduce the intermolecular hydrogen bonding force, has a higher viscosity index, and exhibits good smoothness. The fiber bundling is adjusted by adding mineral oil. Therefore, the fiber smoothness and partial bundling problems are solved by compounding EO / PO random copolymerized lauryl alcohol polyether with mineral oil, and isomeric tridecanol polyoxyethylene ether is introduced. Isomeric tridecanol polyoxyethylene ether is a nonionic surfactant. Nonionic surfactants have high surface activity and excellent wetting properties. Isomeric tridecanol polyoxyethylene ether exhibits excellent emulsifying power, which is that the interfacial film formed by the branching of the hydrophobic group has higher strength, and the formed emulsion is more stable. At the same time, its HLB value is small, that is, the hydrophilic-lipophilic balance value is small.

[0024] 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 and hydroxyl groups in fiber macromolecules to form strong directional adsorption, which can improve the wear resistance of fibers, reduce the hair caused by fiber breakage during the spinning process, and improve the processability of fibers;

[0025] 4) The preparation method of amino silicone oil has good controllability and good reaction stability. DETAILED DESCRIPTION

[0026] The present invention is further described below in conjunction with embodiments.

[0027] An embodiment of the present invention provides a fully matte polyester fiber, wherein the fully matte polyester fiber contains titanium dioxide, and the oil agent used for oiling the fully matte polyester fiber includes at least isotridecyl alcohol polyoxyethylene ether. The oil agent containing isotridecyl alcohol polyoxyethylene ether can adjust the static friction coefficient and the dynamic friction coefficient to obtain suitable cohesion of the fiber, solve the problem of poor cohesion due to high titanium dioxide content, and avoid filament damage, filament tripping, floating filaments and lint. Isotridecyl alcohol polyoxyethylene ether is a non-ionic surfactant with high surface activity and excellent wetting properties. Isotridecyl alcohol polyoxyethylene ether exhibits excellent emulsifying power, in that the interfacial film formed by hydrophobic group branching has higher strength and the formed emulsion is more stable. At the same time, its HLB value is small, that is, the hydrophilic-lipophilic balance value is small. After testing, isotridecyl alcohol polyoxyethylene ether is most conducive to the formation of fibers.

[0028] In some embodiments, the content of titanium dioxide is 2.0-2.2wt%. When the content of titanium dioxide is higher than 2.2wt%, the matting effect is not obvious and the friction force is greatly increased. When the content of titanium dioxide is less than 2.0wt%, the matting effect is not obvious. Titanium dioxide is added in the form of masterbatch, mixed, melted and extruded by a screw.

[0029] In some embodiments, the oil agent is calculated by weight, and the contents of each component are as follows: 30-40 parts of EO / PO random copolymer lauryl alcohol polyether, 30-40 parts of mineral oil, 15-20 parts of isomeric tridecyl alcohol polyoxyethylene ether, 8-10 parts of amino silicone oil, and 8-15 parts of fatty alcohol polyoxyethylene ether potassium salt.

[0030] The performance change trend of the main components of the oil agent from mineral oil, fatty alcohol, polyol ester to polyether is that the bundling of the filaments changes from good to poor, and the film strength changes from poor to strong. EO / PO random copolymerized lauryl alcohol polyether, which is polymerized by ethylene oxide and propylene oxide, has the advantages of good viscosity-temperature performance, high temperature resistance and less smoke, and is used as a lubricant for the oil agent. Among them, EO / PO random copolymerized lauryl alcohol polyether can reduce the intermolecular hydrogen bond force due to the alternating distribution of EO / PO, has a higher viscosity index, and shows good smoothness, but the single EO / PO random copolymerized lauryl alcohol polyether has poor bundling of the filaments and is difficult to meet the requirements of the cohesion of the full matte fiber. Therefore, the inventor adjusts the bundling of the fiber by adding mineral oil. Mineral oil is cheap, has good smoothness at low temperatures, and has good sizing properties. At the same time, the heat resistance and oil film strength of mineral oil are weaker than those of polyether. Therefore, the problems of fiber smoothness and partial bundling are solved by compounding EO / PO random copolymer lauryl alcohol polyether with mineral oil.

[0031] On the basis of solving the fiber smoothness and partial clustering, the inventor introduces isomeric tridecanol polyoxyethylene ether, which is a nonionic surfactant, and the nonionic surfactant has very high surface activity and excellent wetting properties. The wetting property determines the wetting, spreading, penetration and diffusion speed of the oil agent on the fiber surface, and ensures that the oil agent can be evenly attached to the silk very quickly during the high-speed spinning process. Isomeric tridecanol polyoxyethylene ether shows excellent emulsifying power, and the interfacial film strength formed by the branching of the hydrophobic group is higher, and the emulsion formed is more stable, and its HLB value is small, that is, the hydrophilic-lipophilic balance value is small, so that the spinning oil agent has good wettability. Isomeric tridecanol polyoxyethylene ether has higher stability and compatibility in aqueous solution, is conducive to improving the smoothness of the oil agent, and has good wettability, spreading and permeability.

[0032] Specifically, the isomeric tridecanol polyoxyethylene ether is one of isomeric tridecanol polyoxyethylene ether 1303, 1305, and 1306, the potassium phosphate is dodecyl phosphate potassium salt or dodecanol phosphate potassium salt, and the fatty alcohol polyoxyethylene ether phosphate potassium salt serves as an antistatic agent and has an antistatic effect.

[0033] The present invention also provides a method for preparing a fully matte polyester fiber, comprising the following steps: preparing the oil agent, metering the fully matte polyester, extruding it to obtain a fully matte polyester melt, cooling it, oiling it with the oil agent, pre-networking it, and winding it to prepare the fully matte polyester fiber, wherein the characteristic viscosity of the fully matte polyester melt is 0.615-0.630dL / g.

[0034] In some embodiments, the steps of preparing the oil agent are as follows: prepare amino silicone oil, mix EO / PO random copolymer lauryl alcohol polyether, isomeric tridecanol polyoxyethylene ether, the amino silicone oil and fatty alcohol polyoxyethylene ether phosphate potassium salt evenly, add them to the mineral oil and stir evenly to obtain the oil agent, the mixing is carried out at room temperature, the stirring temperature is 40-55°C, and the time is 1-3h. When the oil agent is used, it is prepared into an emulsion with a concentration of 10-12wt% with water.

[0035] In some embodiments, the steps for preparing the aminosilicone oil are as follows: adding hydrogen-containing silicone oil, a catalyst, and toluene into a reaction vessel, 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 the catalyst is 0.015-0.020% by weight of the hydrogen-containing silicone oil, the acrylamine titration time is 1.5-2h, the reaction temperature in the reaction vessel is 60-80°C, after reacting for 1-1.5h, adding excess n-propanol, which is conducive to dissolution and purification, stirring for 1-1.5h, and the reaction product is subjected to reduced pressure distillation to remove the solvent and the remaining acrylamine and n-propanol to obtain the aminosilicone oil, the catalyst is selected from chloroplatinic acid, and the preparation method of the aminosilicone oil has good controllability and good reaction stability.

[0036] 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 groups, hydroxyl groups, etc. in fiber macromolecules to form strong directional adsorption, which can improve the wear resistance of fibers, reduce the fuzz caused by fiber breakage during the spinning process, and improve the processability of fibers.

[0037] Specifically, the viscosity of the hydrogen-containing silicone oil is 50-100 mPa·s, and the structural formula of the hydrogen-containing silicone oil is:

[0038]

[0039] Wherein, x is a positive integer from 3 to 120.

[0040] In some embodiments, the oil film strength of the oil agent is 107-115kg, the surface tension of the oil agent is 31.8-33.2cN / cm, the wetting time is 2.0-2.5s, and after the full-dull polyester fiber is oiled with the oil agent, the static friction coefficient between the full-dull polyester fibers is 0.297-0.305, and the dynamic friction coefficient is 0.286-0.293.

[0041] The difference between the static friction coefficient μs and the dynamic friction coefficient μd has a great influence on the cohesion and smoothness, and the oil agent needs both to be excellent and suitable. For DTY processing to obtain excellent cohesion, the static friction coefficient μs of the fiber must be greater than the dynamic friction coefficient μd, and at the same time ensure that the difference is within a certain range. When μs-μd is equal, the smoothness and cohesion cannot meet the requirements of spinning, and polyether and mineral oil are selected as the main components of the smoothing agent. Polyether can reduce the static friction coefficient μs between fibers, which is beneficial to elasticization, but increases the dynamic friction coefficient μd between fibers and metals, which is not conducive to stretching. Mineral oil increases the static friction coefficient between fibers and reduces the dynamic friction coefficient μd between fibers and metals. The present invention selects isomeric tridecanol polyoxyethylene ether, amino silicone oil, polyether, mineral oil and isomeric tridecanol polyoxyethylene ether. More importantly, the suitable cohesion of the fiber is obtained 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 0.297-0.305, the dynamic friction coefficient is 0.286-0.293, the difference between the static friction coefficient μs and the dynamic friction coefficient μd is appropriate, and the fibers are smooth and excellent in adhesion.

[0042] In some embodiments, the extrusion temperature of the fully matte polyester is 280-290°C, the cooling air temperature of the fully matte polyester is 20-25°C, the pre-network pressure is 0.03±0.005Mpa, the pre-network is before winding to prevent the fully matte polyester fiber from loosening, the winding speed of the fully matte polyester is 2500-3000m / min, and the fully matte polyester fiber prepared under suitable reaction conditions has good mechanical properties. The fully matte polyester fiber has a fineness of 75-150dtex, a breaking strength of ≥1.8cN / dtex, an elongation at break of 120.0±10.0%, a linear density deviation rate of ≤1.2%, a breaking strength CV value of ≤5.0%, a breaking elongation CV value of ≤5.0%, and a yarn dryness CV of ≤1.10%.

[0043] Example 1

[0044] A fully matte polyester fiber, the fully matte polyester fiber contains titanium dioxide, the oil agent used for oiling the fully matte polyester fiber comprises at least isotridecyl alcohol polyoxyethylene ether, the content of the titanium dioxide is 2.0wt%, and the content of each component of the oil agent is as follows in parts by weight: 30 parts of EO / PO random copolymerized lauryl alcohol polyether, 30 parts of mineral oil, 15 parts of isotridecyl alcohol polyoxyethylene ether, 8 parts of amino silicone oil, and 8 parts of potassium salt of fatty alcohol polyoxyethylene ether phosphate, the isotridecyl alcohol polyoxyethylene ether is isotridecyl alcohol polyoxyethylene ether 1303, and the mineral oil is cosmetic grade mineral white oil (Hangzhou Fuda Petrochemical Co., Ltd.).

[0045] A method for preparing a fully matte polyester fiber comprises the following steps: preparing the oil agent, metering the fully matte polyester, extruding the fully matte polyester to obtain a fully matte polyester melt, cooling, oiling with the oil agent, pre-networking, and winding to prepare the fully matte polyester fiber, wherein the fully matte polyester melt has a characteristic viscosity of 0.615 dL / g.

[0046] The steps of preparing the oil agent are as follows: preparing amino silicone oil, mixing EO / PO random copolymerized lauryl alcohol polyether, isomeric tridecanol polyoxyethylene ether 1303, the amino silicone oil and fatty alcohol polyoxyethylene ether phosphate potassium salt evenly, adding them into the mineral oil and stirring evenly to obtain the oil agent, the mixing is carried out at room temperature, the stirring temperature is 40°C, and the stirring time is 1 hour. When the oil agent is used, it is prepared into an emulsion with a concentration of 10wt% with water.

[0047] The steps of preparing the amino silicone oil are as follows: adding hydrogen-containing silicone oil, a catalyst, and toluene into a reaction vessel, and dripping acrylamine 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 the catalyst is 0.015% of the weight of the hydrogen-containing silicone oil, the acrylamine titration time is 1.5h, the reaction temperature in the reaction vessel is 60°C, after reacting for 1h, adding excess n-propanol within 30min, stirring for 1h, and removing the solvent and the remaining acrylamine and n-propanol from the reaction product by reduced pressure distillation to obtain the amino silicone oil, wherein the catalyst is chloroplatinic acid, the viscosity of the hydrogen-containing silicone oil is 50mPa·s, and the structural formula of the hydrogen-containing silicone oil is:

[0048]

[0049] In the formula, x is 3.

[0050] The oil film strength of the oil agent measured by MR8-10 four-ball friction tester is 107 kg.

[0051] The surface tension of the oil is 31.8 cN / cm, and the surface tension is measured by a JZHY1-80 surface tension meter under the conditions of 1% concentration and 30 degrees Celsius temperature.

[0052] Prepare 1% oil emulsion, heat to 30℃, wait for the foam to disappear, place the canvas flat on the emulsion surface, start timing, and record the time when the canvas is completely wetted and starts to sink as the wetting time. The measured wetting time is 2.0s.

[0053] The friction coefficient test adopts the Rode method, the instrument is R-180 filament friction coefficient meter, the speed v=0.5m / min, the angle ψ=4×360°, and after the full-dull polyester fiber is oiled with the oil agent, the static friction coefficient between the full-dull polyester fibers is measured to be 0.297, and the dynamic friction coefficient is 0.286.

[0054] The extrusion temperature of the full-dull polyester is 280° C., the cooling air temperature of the full-dull polyester is 20° C., the pre-network pressure is 0.032 MPa, and the winding speed of the full-dull polyester is 2500 m / min;

[0055] The test results show that the fineness of the full-dull polyester fiber is 75 dtex, the breaking strength is 2.06 cN / dtex, the breaking elongation is 122.0%, the linear density deviation rate is 1.06%, the breaking strength CV value is 4.82%, the breaking elongation CV value is 4.75%, and the yarn dryness CV is 1.02%.

[0056] Example 2

[0057] A fully matte polyester fiber, the fully matte polyester fiber contains titanium dioxide, the oil agent used for oiling the fully matte polyester fiber comprises at least isotridecyl alcohol polyoxyethylene ether, the content of the titanium dioxide is 2.1wt%, and the content of each component of the oil agent is as follows by weight: 35 parts of EO / PO random copolymerized lauryl alcohol polyether, 35 parts of mineral oil, 17 parts of isotridecyl alcohol polyoxyethylene ether, 9 parts of amino silicone oil, and 10 parts of fatty alcohol polyoxyethylene ether potassium phosphate, the isotridecyl alcohol polyoxyethylene ether is isotridecyl alcohol polyoxyethylene ether 1305, and the potassium phosphate is dodecaethanol potassium phosphate.

[0058] A method for preparing a fully matte polyester fiber comprises the following steps: preparing the oil agent, metering the fully matte polyester, extruding the fully matte polyester to obtain a fully matte polyester melt, cooling, oiling with the oil agent, pre-networking, and winding to prepare the fully matte polyester fiber, wherein the fully matte polyester melt has a characteristic viscosity of 0.62 dL / g.

[0059] The steps of preparing the oil agent are as follows: preparing amino silicone oil, mixing EO / PO random copolymerized lauryl alcohol polyether, isomeric tridecanol polyoxyethylene ether 1305, the amino silicone oil and fatty alcohol polyoxyethylene ether phosphate potassium salt evenly, adding them into the mineral oil and stirring evenly to obtain the oil agent, the mixing is carried out at room temperature, the stirring temperature is 50°C, and the stirring time is 2h. When the oil agent is used, it is prepared into an emulsion with a concentration of 11wt% with water.

[0060] The steps of preparing the amino silicone oil are as follows: adding hydrogenated silicone oil, a catalyst and toluene into a reaction vessel, and dropping acrylamine under stirring, wherein the molar ratio of acrylamine to the hydrogen content in the hydrogenated silicone oil is 1.0:1.1, the mass ratio of toluene to the hydrogenated silicone oil is 1.0:0.9, the amount of the catalyst is 0.018% of the weight of the hydrogenated silicone oil, the acrylamine titration time is 1.5h, the reaction temperature in the reaction vessel is 70°C, after the reaction time is 1.2h, adding excess n-propanol within 30min, stirring for 1.2h, and removing the solvent and the remaining acrylamine and n-propanol from the reaction product by reduced pressure distillation to obtain the amino silicone oil, wherein the catalyst is chloroplatinic acid, the viscosity of the hydrogenated silicone oil is 80mPa·s, and the structural formula of the hydrogenated silicone oil is:

[0061]

[0062] In the formula, x is 68.

[0063] The oil film strength of the oil agent measured by MR8-10 four-ball friction tester is 110 kg.

[0064] The surface tension of the oil is 32.5 cN / cm, and the surface tension is measured by a JZHY1-80 surface tension meter under the conditions of 1% concentration and 30 degrees Celsius temperature.

[0065] Prepare 1% oil emulsion, heat to 30℃, wait for the foam to disappear, place the canvas flat on the emulsion surface, start timing, and record the time when the canvas is completely wetted and starts to sink as the wetting time. The measured wetting time is 2.2s.

[0066] The friction coefficient test adopts the Rode method, the instrument is R-180 filament friction coefficient meter, the speed v=0.5m / min, the angle ψ=4×360°, and after the full-dull polyester fiber is oiled with the oil agent, the static friction coefficient between the full-dull polyester fibers is measured to be 0.300, and the dynamic friction coefficient is 0.291.

[0067] The extrusion temperature of the full-dull polyester is 285° C., the cooling air temperature of the full-dull polyester is 22° C., the pre-network pressure is 0.03 Mpa, and the winding speed of the full-dull polyester is 2800 m / min;

[0068] The test results show that the fineness of the fully matte polyester fiber is 100 dtex, the breaking strength is 2.03 cN / dtex, the breaking elongation is 125.0%, the linear density deviation rate is 0.94%, the breaking strength CV value is 4.76%, the breaking elongation CV value is 4.81%, and the yarn CV is 0.92%.

[0069] Example 3

[0070] A fully matte polyester fiber, the fully matte polyester fiber contains titanium dioxide, the oil agent used for oiling the fully matte polyester fiber comprises at least isotridecyl alcohol polyoxyethylene ether, the content of the titanium dioxide is 2.2wt%, and the content of each component of the oil agent is as follows in parts by weight: 40 parts of EO / PO random copolymerized lauryl alcohol polyether, 40 parts of mineral oil, 20 parts of isotridecyl alcohol polyoxyethylene ether, 10 parts of amino silicone oil, and 15 parts of fatty alcohol polyoxyethylene ether potassium phosphate, the isotridecyl alcohol polyoxyethylene ether is isotridecyl alcohol polyoxyethylene ether 1306, and the potassium phosphate is dodecaethanol potassium phosphate.

[0071] A method for preparing a fully matte polyester fiber comprises the following steps: preparing the oil agent, metering the fully matte polyester, extruding the fully matte polyester to obtain a fully matte polyester melt, cooling, oiling with the oil agent, pre-networking, and winding to prepare the fully matte polyester fiber, wherein the fully matte polyester melt has a characteristic viscosity of 0.63 dL / g.

[0072] The steps of preparing the oil agent are as follows: prepare amino silicone oil, mix EO / PO random copolymerized lauryl alcohol polyether, isomeric tridecanol polyoxyethylene ether 1306, the amino silicone oil and fatty alcohol polyoxyethylene ether phosphate potassium salt evenly, add them into the mineral oil and stir evenly to obtain the oil agent, the mixing is carried out at room temperature, the stirring temperature is 55°C, and the stirring time is 3 hours. When the oil agent is used, it is prepared into an emulsion with a concentration of 12wt% with water.

[0073] The steps of preparing the amino silicone oil are as follows: adding hydrogenated silicone oil, a catalyst and toluene into a reaction vessel, and dropping acrylamine under stirring, wherein the molar ratio of acrylamine to the hydrogen content in the hydrogenated silicone oil is 1.0:1.1, the mass ratio of toluene to the hydrogenated silicone oil is 1.0:0.9, the amount of the catalyst is 0.020% of the weight of the hydrogenated silicone oil, the acrylamine titration time is 2 hours, the reaction temperature in the reaction vessel is 80°C, after the reaction time is 1.5 hours, adding excess n-propanol within 30 minutes, stirring for 1.5 hours, and removing the solvent and the remaining acrylamine and n-propanol from the reaction product by reduced pressure distillation to obtain the amino silicone oil, wherein the catalyst is chloroplatinic acid, the viscosity of the hydrogenated silicone oil is 100 mPa·s, and the structural formula of the hydrogenated silicone oil is:

[0074]

[0075] Where x is 120.

[0076] The oil film strength of the oil agent measured by MR8-10 four-ball friction tester is 115 kg.

[0077] The surface tension of the oil is 33.2 cN / cm, and the surface tension is measured by a JZHY1-80 surface tension meter under the conditions of 1% concentration and 30 degrees temperature.

[0078] Prepare 1% oil emulsion, heat to 30℃, wait for the foam to disappear, place the canvas flat on the emulsion surface, start timing, and record the time when the canvas is completely wetted and starts to sink as the wetting time. The measured wetting time is 2.5s.

[0079] The friction coefficient test adopts the Rode method, the instrument is R-180 filament friction coefficient meter, the speed v=0.5m / min, the angle ψ=4×360°, and after the full-dull polyester fiber is oiled with the oil agent, the static friction coefficient between the full-dull polyester fibers is measured to be 0.305, and the dynamic friction coefficient is 0.293.

[0080] The extrusion temperature of the full-dull polyester is 290° C., the cooling air temperature of the full-dull polyester is 25° C., the pre-network pressure is 0.035 MPa, and the winding speed of the full-dull polyester is 3000 m / min;

[0081] The test results show that the fineness of the full-dull polyester fiber is 150 dtex, the breaking strength is 1.97 cN / dtex, the breaking elongation is 130.0%, the linear density deviation rate is 0.98%, the breaking strength CV value is 4.72%, the breaking elongation CV value is 4.77%, and the yarn CV is 0.96%.

[0082] The fully matte polyester fibers coated with oil in Examples 1, 2 and 3 have reasonable cohesion, and will not produce hairy, tripped or floating fibers during production. The fully matte polyester fibers have excellent mechanical properties.

[0083] 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.

[0084] Unless otherwise specified, 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.

[0085] 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.

[0086] 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.

[0087] 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 fully matte polyester fiber, characterized in that: The fully matte polyester fiber contains titanium dioxide, and the oiling agent used for oiling the fully matte polyester fiber at least includes isomeric tridecanol polyoxyethylene ether.

2. The full matte polyester fiber according to claim 1, characterized in that: The content of titanium dioxide is 2.0-2.2 wt %.

3. The full matte polyester fiber according to claim 1, characterized in that: The oil agent has the following components in parts by weight: 30-40 parts of EO / PO random copolymerized lauryl alcohol polyether, 30-40 parts of mineral oil, 15-20 parts of isomeric tridecanol polyoxyethylene ether, 8-10 parts of amino silicone oil, and 8-15 parts of potassium salt of fatty alcohol polyoxyethylene ether phosphate.

4. The full matte polyester fiber according to claim 3, characterized in that: The isomeric tridecanol polyoxyethylene ether is one of isomeric tridecanol polyoxyethylene ether 1303, 1305, and 1306.

5. The method for preparing the fully matte polyester fiber according to any one of claims 1 to 4, characterized in that: The following steps are involved: The oil agent is prepared, and the fully matte polyester is metered, melted, extruded to obtain a fully matte polyester melt, cooled, oiled with the oil agent, pre-networked, and wound to prepare the fully matte polyester fiber. The characteristic viscosity of the fully matte polyester melt is 0.615-0.630dL / g.

6. The method for preparing the fully matte polyester fiber according to claim 5, characterized in that: The steps of preparing the oil agent are as follows: prepare amino silicone oil, mix EO / PO random copolymerized lauryl alcohol polyether, isomeric tridecanol polyoxyethylene ether, the amino silicone oil and fatty alcohol polyoxyethylene ether phosphate potassium salt evenly, add them into the mineral oil and stir evenly to obtain the oil agent, and the mixing is carried out at room temperature, the stirring temperature is 40-55°C, and the time is 1-3h.

7. The method for preparing the fully matte polyester fiber according to claim 6, characterized in that: The steps for preparing the amino silicone oil are as follows: adding hydrogen-containing silicone oil, a catalyst 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 the catalyst is 0.015-0.020% of the weight of the hydrogen-containing silicone oil, the acrylamine titration time is 1.5-2h, the reaction temperature in the reaction container is 60-80°C, after reacting for 1-1.5h, adding excess n-propanol, stirring for 1-1.5h, and removing the solvent and the remaining acrylamine and n-propanol from the reaction product by reduced pressure distillation to obtain the amino silicone oil, and the catalyst is chloroplatinic acid.

8. The method for preparing the fully matte polyester fiber according to claim 7, characterized in that: The viscosity of the hydrogen-containing silicone oil is 50-100 mPa·s, and the structural formula of the hydrogen-containing silicone oil is: Wherein, x is a positive integer from 3 to 120.

9. The method for preparing the fully matte polyester fiber according to any one of claims 5 to 8, characterized in that: The oil film strength of the oil agent is 107-115kg, the surface tension of the oil agent is 31.8-33.2cN / cm, the wetting time is 2.0-2.5s, and after the full-dull polyester fiber is oiled with the oil agent, the static friction coefficient between the full-dull polyester fibers is 0.297-0.305, and the dynamic friction coefficient is 0.286-0.

293.

10. The method for preparing the fully matte polyester fiber according to claim 5, characterized in that: The extrusion temperature of the full-dull polyester is 280-290° C., the cooling air temperature of the full-dull polyester is 20-25° C., the pre-network pressure is 0.03±0.005Mpa, and the winding speed of the full-dull polyester is 2500-3000m / min; The full-dull polyester fiber has a fineness of 75-150 dtex, a breaking strength of ≥1.8 cN / dtex, a breaking elongation of 120.0±10.0%, a linear density deviation rate of ≤1.2%, a breaking strength CV value of ≤5.0%, a breaking elongation CV value of ≤5.0%, and a yarn evenness CV of ≤1.10%.

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