Modified polyester yarn suitable for water-jet weaving and light sizing and preparation method of modified polyester yarn
By grafting DOPO-HEMA onto polyester yarn and subjecting it to corona treatment, combined with nano-hybrid sizing materials, the problems of yarn breakage, entanglement, insufficient strength, and poor flame retardancy in the water-jet weaving process of polyester yarn are solved, achieving a light sizing effect with high strength, abrasion resistance, and good flame retardancy.
Patent Information
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2025-12-18
- Publication Date
- 2026-03-13
AI Technical Summary
Existing polyester yarns suffer from problems such as breakage, entanglement, poor fiber cohesion, insufficient strength, poor hydrophobicity and adsorption to traditional sizing agents, and insufficient flame retardancy during water jet weaving.
DOPO-HEMA grafted modified polyester yarn is used, and after ultraviolet light irradiation and corona treatment, it is lightly sized with nano-hybrid material sizing to form a gradient functionalized structure, which improves the flame retardancy, abrasion resistance and film strength of the yarn.
It improves the flame retardancy, abrasion resistance and film strength of polyester yarn, reduces hairiness, enhances the cohesion between fibers, and improves the adhesion and desizing performance of the sizing agent.
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Figure CN121653955A_ABST
Abstract
Description
Technical Field
[0001] This invention belongs to the field of textile technology, specifically relating to a modified polyester yarn suitable for water-jet weaving with light sizing and its preparation method. Background Technology
[0002] The water jet loom is a shuttleless loom that uses a high-pressure water jet as the weft insertion medium, drawing the weft yarn from one side of the loom to the other to complete the interlacing of warp and weft yarns. The technical advantages of water jet loom weaving result in good economic efficiency, and as a high-speed shuttleless loom, it has demonstrated strong vitality in the modern textile industry. At the same time, it has also spurred the development of water jet loom sizing agents. Unlike conventional sizing agents, water jet loom sizing agents must meet the following characteristics: easy solubility in water during preparation, water resistance during weaving, and easy removal during desizing.
[0003] Polyester yarn has a lot of surface hair, which easily leads to breakage and tangling during weaving, poor cohesion between fibers, insufficient yarn strength, and poor adsorption of traditional sizing agents due to its hydrophobicity. Water jet looms rely on the lubrication of water for weft insertion, but polyester has a low water absorption rate. At the same time, the sizing film needs to be flexible and wear-resistant, requiring optimization of the sizing agent formula. In addition, polyester has poor flame retardancy. Therefore, there is an urgent need for a modified polyester yarn suitable for water jet weaving with light sizing, which has high sizing film strength, strong wear resistance, and good flame retardancy. Summary of the Invention
[0004] The purpose of this invention is to provide a modified polyester yarn suitable for water-jet weaving and light sizing, and a method for preparing the same, in order to solve the technical problems in the prior art.
[0005] To achieve the above objectives, the present invention adopts the following technical solution:
[0006] This invention provides a method for preparing modified polyester yarn suitable for water-jet weaving and light sizing, comprising the following steps:
[0007] Step (1) Immerse the polyester yarn in an aqueous solution containing DOPO-HEMA and a photoinitiator, heat it, take it out and squeeze it, then irradiate it with ultraviolet light, wash it, and dry it to obtain grafted polyester yarn.
[0008] In the above process, UV irradiation chemical grafting modification is used to graft DOPO-HEMA onto polyester yarn.
[0009] Step (2) After corona treatment of the grafted polyester yarn, the nano-hybrid material slurry is used to sizing the grafted polyester yarn to obtain a modified polyester yarn suitable for light sizing in water jet weaving; the nano-hybrid material slurry specifically includes the following components by weight: 35-45 parts of water-soluble polyester, 50-65 parts of polyacrylate-SiO2 nano-hybrid slurry, 0.5-1 parts of penetrant, and 0.8-1.5 parts of antistatic agent.
[0010] Preferably, in step (1), the polyester yarn is a lightly twisted polyester staple fiber yarn with a yarn count of 10s, 16s, or 21s; the bath ratio of the polyester yarn to the aqueous solution is 1:(5-15); the DOPO-HEMA content is 35-45wt%; the photoinitiator is Ir-2959; the photoinitiator content is 3wt%; the heating conditions are: heating temperature of 55-65℃ and heating time of 1.5-2.5h; the extrusion degree is to extrude to a liquid retention rate of 110-130wt%; the ultraviolet irradiation method is: wrap with cellophane to isolate air, fix it between two glass plates, and irradiate both sides under 365nm ultraviolet light at a distance of 15cm for 8-12min each; the washing method is: wash with distilled water at 75-85℃ for 4-6h; the drying method is: dry at 55-65℃ to constant weight.
[0011] Preferably, the method for preparing the DOPO-HEMA includes the following steps:
[0012] DOPO was added to tetrahydrofuran, carbon tetrachloride was added in an ice-water bath, and after the reaction, triethylamine was added, followed by slow dropwise addition of hydroxyethyl methacrylate (HEMA). After the addition was complete, the temperature was raised and stirring was continued until the reaction was stopped. Impurities were removed, the mixture was dried, filtered, and the solvent was evaporated to obtain DOPO-HEMA.
[0013] The structural formula of DOPO-HEMA is as follows:
[0014]
[0015] Preferably, the ratio of DOPO, tetrahydrofuran, carbon tetrachloride, triethylamine, and hydroxyethyl methacrylate is 21.6-30g:200-300mL:110-165mL:13.2-20g:15.6-23.4g; the reaction time is 9-14min; the heating temperature is 35-40℃; the stirring time is 3-6h; the impurity removal method is vacuum filtration, and the filtrate is washed 3-5 times successively with 3% NaOH solution, distilled water, and saturated NaCl aqueous solution; the drying method is to dry the organic layer with anhydrous MgSO4 overnight.
[0016] Preferably, in step (2), the sizing method is as follows: the grafted polyester yarn is immersed in the nano-hybrid material sizing solution, and sizing is carried out under the conditions of sizing tank temperature of 40-50℃, desizing temperature of 100-105℃, and sizing speed of 30-60m / min; the sizing rate relative to the dry weight of the yarn is 2-4%; the corona treatment conditions are: corona treatment voltage of 8-10kV, corona treatment time of 5-10s; the penetrant is JFC; and the antistatic agent is SK-E.
[0017] Preferably, the preparation method of the polyacrylate-SiO2 nano-hybrid slurry includes the following steps:
[0018] S1: Add nano-silica to methanol, heat and stir, then slowly add silane coupling agent, continue stirring, wash, and dry to obtain silanized nano-silica;
[0019] S2: Diphenylphosphoric acid was dissolved in anhydrous ethanol and stirred to obtain a diphenylphosphoric acid solution; cytosine was dissolved in deionized water and stirred to obtain a cytosine solution; the diphenylphosphoric acid solution and the cytosine solution were mixed and stirred again, then silanized nano-silica was added, the reaction was continued, filtered, and washed to obtain modified nano-SiO2;
[0020] In the above process, the hydroxyl group of diphenyl phosphate first reacts with the amino group of cytosine to obtain a salt of diphenyl phosphate and cytosine, and then the remaining amino group (—NH—) or hydroxyl group (—OH) nucleophilically attacks the epoxy group to undergo a ring-opening reaction, thus obtaining modified nano-SiO2.
[0021] The structural formulas of the salts of diphenyl phosphate and cytosine are as follows:
[0022]
[0023] Mass spectrometry analysis was performed on the salts of diphenylphosphate and cytosine, with HRMS (ESI) m / z values of 220.07 (100.0%), 221.07 (13.2%), and 222.07 (1.2%).
[0024] S3: Modified nano-SiO2 is added to ethanol and ultrasonically treated to obtain nano-SiO2 dispersion. Then, polyacrylate slurry is added, stirred, and ultrasonically treated to obtain polyacrylate-SiO2 nano-hybrid slurry.
[0025] Preferably, in step S1, the ratio of nano-silica, methanol, and silane coupling agent is 50-75g:5-7.5L:10-15mL; the heating and stirring conditions are: heating and stirring temperature is 65-75℃, heating and stirring time is 10-15min; the silane coupling agent is KH-560; the stirring time is continued for 3-5h; the washing method is: washing with methanol and deionized water 3-5 times respectively.
[0026] Preferably, in step S2, the ratio of diphenylphosphoric acid, anhydrous ethanol, cytosine, deionized water, and silanized nano-silica is 65.5-98.3g:2-3L:333.3-500g:2-3L:10-15g; the stirring time is 10-20min; the re-stirring time is 5-10min; the conditions for continued stirring are: the temperature for continued stirring is 65-75℃, the stirring time for continued stirring is 3-5h, and the reaction time for continued reaction is 3-5h.
[0027] Preferably, in step S3, the ratio of modified nano-SiO2, ethanol, and polyacrylate slurry is 10-15:250-370:210-315; the ultrasonic treatment conditions are: ultrasonic power of 200-300W and ultrasonic treatment time of 15-20min; the stirring treatment conditions are: stirring temperature of 90-100℃ and stirring time of 1-1.5h; and the ultrasonic treatment time is 15-25min.
[0028] Preferably, the method for preparing polyacrylate slurry includes the following steps:
[0029] Deionized water, sodium dodecylbenzenesulfonate, sodium dodecyl sulfate, methyl acrylate, and butyl acrylate are mixed and stirred to obtain a mixture. Then, acrylic acid, acrylamide, water, and ammonium persulfate are added dropwise to the mixture, and stirring is continued. The mixture is heated, stirred, and kept at the temperature before being cooled. Ammonia water is added dropwise to neutralize the mixture, and the mixture is filtered to obtain a polyacrylate slurry.
[0030] Preferably, the ratio of deionized water, sodium dodecylbenzenesulfonate, sodium dodecyl sulfate, methyl acrylate, butyl acrylate, acrylic acid, acrylamide, water, and ammonium persulfate is 2-4L:20-40g:10-20g:60-120g:530-1060g:260-520g:450-900g:100-200g:40-80g; the stirring conditions are: stirring temperature of 55-65℃, stirring time of 40-60min; the method for continued stirring is: stirring at 70-80℃ at a speed of 100-140r / min for 1.5-2.5h; the heating temperature is 82-95℃; the stirring and holding time is 0.5-1.5h; the cooling temperature is 40-50℃; and the ammonia concentration is 28wt%.
[0031] The modified polyester yarn suitable for light sizing in water-jet weaving was prepared by the method described above.
[0032] In summary, due to the adoption of the above technical solution, the beneficial effects of the present invention are:
[0033] 1. This invention grafts DOPO-HEMA onto polyester yarn. By initiating the grafting of the phosphorus-containing flame-retardant monomer DOPO-HEMA onto the polyester surface using ultraviolet light, it solves the problems of easy migration and poor durability of traditional flame retardants. DOPO provides highly efficient phosphorus-based flame retardancy, and the cross-linked network formed after HEMA polymerization can promote char formation and isolate heat and oxygen. The modified polyester forms an expanded char layer during combustion, reducing molten dripping. A multi-mode flame-retardant system is formed by DOPO and SiO2, which forms a heat insulation barrier.
[0034] 2. In this invention, the surface is further activated by corona treatment and etched to increase roughness and improve the adhesion of subsequent nano-slurry. Corona treatment, as an intermediate step, can control the degree of activation and avoid excessive damage to the polyester substrate. The slurry combines with the corona-activated DOPO-HEMA layer to form a gradient functionalized structure of polyester, flame retardant layer, and nano-reinforcing layer. The added silica improves the wear resistance of the slurry film. KH560 modified SiO2 crosslinks with the active groups in the slurry through siloxane bonds (-Si-O-) to form a dense nano-coating.
[0035] 3. In this invention, the phenyl groups of DOPO-HEMA enhance the compatibility of SiO2 with the organic phase; the amino / carbonyl groups of cytosine can form hydrogen bonds with the carboxyl or amide groups of polyacrylate, enhancing the dispersibility of modified nano-SiO2 in polyacrylate; the polyester yarn lightly sized with nano-hybrid sizing agent has high sizing film strength, strong abrasion resistance, low viscosity, high yarn breaking strength, reduced hair count, and good desizing performance. Attached Figure Description
[0036] To more clearly illustrate the technical solutions in the embodiments of the present invention or the prior art, the drawings used in the description of the embodiments or the prior art will be briefly introduced below. Obviously, the drawings described below are only some embodiments of the present invention. For those skilled in the art, other drawings can be obtained based on these drawings without creative effort.
[0037] Figure 1 This is a process flow diagram of the preparation of modified polyester yarn suitable for water-jet weaving and light sizing according to the present invention;
[0038] Figure 2 This is a diagram illustrating the flame retardant properties of the modified polyester yarn for light sizing in water-jet weaving, as described in this invention. Detailed Implementation
[0039] The technical solutions of the embodiments of the present invention will be clearly and completely described below with reference to the accompanying drawings. Obviously, the described embodiments are only some embodiments of the present invention, and not all embodiments. Based on the embodiments of the present invention, all other embodiments obtained by those skilled in the art without creative effort are within the scope of protection of the present invention.
[0040] The substances and sources involved in the following examples and comparative examples are shown in Table 1:
[0041] Table 1
[0042] substance Source / Product Information polyester yarn Yancheng Hengrun Chemical Fiber Co., Ltd., Item Nos. T10, T16, T21 Water-soluble polyester Jinan Tangcai Chemical Products Co., Ltd. Item No. 006 DOPO Changzhou Runqian Biotechnology Co., Ltd. Hydroxyethyl methacrylate Shanghai Aladdin Biochemical Technology Co., Ltd. Diphenylphosphine Chongqing Xingcan Pharmaceutical Technology Co., Ltd. Cytosine Shanghai Xianggeng Technology Development Co., Ltd. Nano silica Nanjing Tianxing New Materials Co., Ltd.
[0043] Example 1
[0044] This embodiment discloses a method for preparing polyacrylate slurry, including the following steps:
[0045] 3L of deionized water, 30g of sodium dodecylbenzenesulfonate, 15g of sodium dodecyl sulfate, 90g of methyl acrylate, and 780g of butyl acrylate were stirred at 60℃ for 50min to obtain a mixture. Then, 390g of acrylic acid, 620g of acrylamide, 150g of deionized water, and 60g of ammonium persulfate were added dropwise to the mixture. The mixture was stirred at 75℃ at 120r / min for 2h. Then, the temperature was raised to 87℃, stirred, and kept at that temperature for 1h. The temperature was lowered to 45℃, and 28wt% ammonia water was added dropwise for neutralization. The mixture was then filtered to obtain a polyacrylate slurry.
[0046] Example 2
[0047] This embodiment discloses a method for preparing a polyacrylate-SiO2 nano-hybrid slurry, including the following steps:
[0048] S1: Add 62g of nano-silica to 6.2L of methanol, heat and stir at 70℃ for 12min, slowly add 13mL of silane coupling agent KH-560, continue stirring for 4h, wash 4 times with methanol and deionized water respectively, and dry to obtain silanized nano-silica.
[0049] S2: Dissolve 81g of diphenylphosphoric acid in 2.5L of anhydrous ethanol and stir for 15min to obtain a diphenylphosphoric acid solution. Dissolve 420g of cytosine in 2.5L of deionized water and stir for 8min to obtain a cytosine solution. Mix the diphenylphosphoric acid solution and the cytosine solution and stir at 70℃ for 4h. Then add 12g of silanized nano-silica and continue the reaction for 4h. Filter and wash to obtain modified nano-SiO2.
[0050] S3: Add 13g of modified nano-SiO2 to 310g of ethanol and sonicate at 250W for 18min to obtain nano-SiO2 dispersion. Then add 256g of polyacrylate slurry prepared in Example 1, stir at 95℃ for 1.2h, and sonicate for 20min to obtain polyacrylate-SiO2 nano-hybrid slurry.
[0051] Example 3
[0052] This embodiment discloses a method for preparing DOPO-HEMA, including the following steps:
[0053] 25g of DOPO was added to 250mL of tetrahydrofuran, and 130mL of carbon tetrachloride was added in an ice-water bath. After reacting for 12min, 16g of triethylamine was added, followed by the slow addition of 19g of hydroxyethyl methacrylate (HEMA). After the addition was complete, the temperature was raised to 38℃ and the mixture was stirred for 4h before the reaction was stopped. The mixture was then filtered under reduced pressure, and the filtrate was washed four times successively with 3% NaOH solution, distilled water, and saturated NaCl aqueous solution. The organic layer was dried overnight with anhydrous MgSO4, filtered, and the solvent was evaporated to obtain DOPO-HEMA.
[0054] Example 4
[0055] See Figure 1 As shown, this embodiment discloses a method for preparing modified polyester yarn suitable for water-jet weaving and light sizing, including the following steps:
[0056] Step (1) The polyester yarn was immersed in an aqueous solution containing 40wt% of DOPO-HEMA prepared in Example 3 and 3wt% Ir-2959 photoinitiator at a bath ratio of 1:10. After heating at 60°C for 2 hours, it was taken out and squeezed to a liquid retention rate of 120wt%. It was wrapped with cellophane to isolate it from the air, sandwiched between two glass plates and fixed. It was then irradiated on both sides for 10 minutes at a distance of 15cm under 365nm ultraviolet light. Then it was washed with distilled water at 80°C for 5 hours and finally dried at 60°C to constant weight to obtain grafted polyester yarn.
[0057] The polyester yarn is a lightly twisted 16s polyester staple fiber yarn.
[0058] Step (2) The grafted polyester yarn is subjected to corona treatment at a voltage of 9kV and a time of 8s. Then, the nano-hybrid material slurry prepared in Example 2 is used to sizing the grafted polyester yarn to obtain a modified polyester yarn suitable for light sizing in water jet weaving.
[0059] The nano-hybrid material slurry specifically comprises the following components by weight: 40 parts water-soluble polyester, 55 parts polyacrylate-SiO2 nano-hybrid slurry, 0.8 parts penetrant JFC, and 1.2 parts antistatic agent SK-E.
[0060] Sizing method: Immerse the grafted polyester yarn in nano-hybrid material sizing, the sizing tank temperature is 45℃, the desizing temperature is 102℃, and the sizing speed is 50m / min; the sizing rate is 3% relative to the dry weight of the yarn.
[0061] Example 5
[0062] See Figure 1 As shown, this embodiment discloses a method for preparing modified polyester yarn suitable for water-jet weaving and light sizing, including the following steps:
[0063] Step (1) The polyester yarn was immersed in an aqueous solution containing 45wt% of DOPO-HEMA prepared in Example 3 and 3wt% Ir-2959 photoinitiator at a bath ratio of 1:5. After heating at 55°C for 2.5h, it was taken out and squeezed to a liquid retention rate of 110wt%. It was wrapped with cellophane to isolate it from the air, fixed between two glass plates, and irradiated on both sides for 12min at a distance of 15cm under 365nm ultraviolet light. Then it was washed with distilled water at 75°C for 6h, and finally dried at 55°C to constant weight to obtain grafted polyester yarn.
[0064] The polyester yarn is 10s lightly twisted polyester staple fiber yarn.
[0065] Step (2) Corona treatment is performed on the grafted polyester yarn under the conditions of 10kV voltage and 5s time. Then, the nano-hybrid material slurry prepared in Example 2 is used to sizing the grafted polyester yarn to obtain modified polyester yarn suitable for water jet weaving with light sizing.
[0066] The nano-hybrid material slurry specifically comprises the following components by weight: 45 parts water-soluble polyester, 50 parts polyacrylate-SiO2 nano-hybrid slurry, 1 part penetrant JFC, and 0.8 parts antistatic agent SK-E.
[0067] Sizing method: Immerse the grafted polyester yarn in nano-hybrid sizing material, the sizing tank temperature is 50℃, the desizing temperature is 100℃, and the sizing speed is 60m / min; the sizing rate is 2% relative to the dry weight of the yarn.
[0068] Example 6
[0069] See Figure 1 As shown, this embodiment discloses a method for preparing modified polyester yarn suitable for water-jet weaving and light sizing, including the following steps:
[0070] Step (1) The polyester yarn was immersed in an aqueous solution containing 35wt% of DOPO-HEMA prepared in Example 3 and 3wt% Ir-2959 photoinitiator at a bath ratio of 1:15. After heating at 65°C for 1.5h, it was taken out and squeezed to a liquid retention rate of 130wt%. It was wrapped with cellophane to isolate it from the air, fixed between two glass plates, and irradiated on both sides for 8min at a distance of 15cm under 365nm ultraviolet light. Then it was washed with distilled water at 85°C for 4h, and finally dried at 65°C to constant weight to obtain grafted polyester yarn.
[0071] The polyester yarn is 21s lightly twisted polyester staple fiber yarn.
[0072] Step (2) Corona treatment is performed on the grafted polyester yarn under the conditions of 8kV voltage and 10s time. Then, the nano-hybrid material slurry prepared in Example 2 is used to sizing the grafted polyester yarn to obtain modified polyester yarn suitable for light sizing in water jet weaving.
[0073] The nano-hybrid material slurry specifically comprises the following components by weight: 35 parts water-soluble polyester, 65 parts polyacrylate-SiO2 nano-hybrid slurry, 0.5 parts penetrant JFC, and 1.5 parts antistatic agent SK-E.
[0074] Sizing method: Immerse the grafted polyester yarn in nano-hybrid sizing material, the sizing tank temperature is 40℃, the desizing temperature is 105℃, the sizing speed is 30m / min; the sizing rate is 4% relative to the dry weight of the yarn.
[0075] Comparative Example 1
[0076] Compared with Example 4, Comparative Example 1 did not have step (1) in the process of preparing modified polyester yarn suitable for water jet weaving and light sizing. That is, in step two, polyester yarn was used to replace grafted polyester yarn, and other conditions remained unchanged.
[0077] Comparative Example 2
[0078] Compared with Example 4, in the process of preparing modified polyester yarn suitable for water jet weaving and light sizing, the composition of the nano-hybrid material slurry in step (2) of Comparative Example 2 was changed. The polyacrylate-SiO2 nano-hybrid slurry was replaced with polyacrylate, and other conditions remained unchanged.
[0079] Comparative Example 3
[0080] Compared with Example 4, in the process of preparing modified polyester yarn suitable for water jet weaving and light sizing, Comparative Example 3 did not perform corona treatment on the grafted polyester yarn in step (2), and all other conditions remained unchanged.
[0081] Experimental Example
[0082] The properties of the modified polyester yarns prepared in Examples 4-6 and Comparative Examples 1-3, suitable for water-jet weaving and light sizing, were tested.
[0083] The breaking strength and elongation at break of the yarn were tested using a YG026 tensile testing machine; the number of abrasion cycles was tested using a single yarn abrasion tester, and the test results are shown in Table 2.
[0084] Table 2
[0085] Group Mean fracture strength / cN Mean elongation at break / % Friction Intensity / % Example 4 1425.65 32.19 53.5 Example 5 1378.72 31.35 52,7 Example 6 1356.48 30.27 50.4 Comparative Example 1 1226.34 25.68 32.6 Comparative Example 2 1151.26 26.97 30.4 Comparative Example 3 1175.91 27.39 30.3
[0086] As can be seen from Table 2, the modified polyester yarns prepared in Examples 4-6, suitable for light sizing in water-jet weaving, have good mechanical properties and abrasion resistance. A comparison between Comparative Example 1 and Example 4 shows that in the preparation of modified polyester yarns suitable for light sizing in water-jet weaving, grafting polyester yarn significantly improves mechanical properties. Without DOPO-HEMA grafting, the crosslinking network provides less additional mechanical strength, and interfacial compatibility decreases. Furthermore, the crosslinked polymer formed after DOPO-HEMA grafting improves surface abrasion resistance. Without grafting, the abrasion resistance decreases solely due to the reinforcing effect of SiO2. Therefore, the absence of DOPO-HEMA grafting leads to a decrease in the mechanical properties of the polyester yarn. Comparative Example 2... Compared with Example 4, it can be seen that in the process of preparing modified polyester yarn suitable for light sizing in water-jet weaving, the polyacrylate-SiO2 nano-hybrid sizing agent of the present invention is replaced with polyacrylate. As rigid particles, SiO2 nanoparticles can disperse stress and hinder molecular chain slippage, which can significantly improve the abrasion resistance and mechanical strength of the coating. Therefore, replacing the polyacrylate-SiO2 nano-hybrid sizing agent with polyacrylate reduces the mechanical properties and abrasion resistance of the polyester yarn. As can be seen from the comparison between Comparative Example 3 and Example 4, in the process of preparing modified polyester yarn suitable for light sizing in water-jet weaving, the grafted polyester yarn is not corona treated, which reduces the adhesion between the sizing agent and the fiber, resulting in a decrease in breaking strength, easy peeling of the sizing agent, and reduced abrasion resistance.
[0087] Vertical burning tests (UL-94) were conducted according to ISO 9773 standard; the limiting oxygen index (%) was tested according to GB / T 2406—1993, and the test results are shown in Table 3.
[0088] Table 3
[0089] Group Limiting Oxygen Index (LOI) / % Number of molten droplets / drop Example 4 34.1 0 Example 5 32.5 0.4 Example 6 33.7 0.2 Comparative Example 1 23.5 3.5 Comparative Example 2 28.1 1.6 Comparative Example 3 32.2 1.3
[0090] As can be seen from Table 3, the modified polyester yarns suitable for light sizing in water-jet weaving prepared in Examples 4-6 have good flame retardancy. A comparison between Comparative Example 1 and Example 4 shows that in the preparation of the modified polyester yarns suitable for light sizing in water-jet weaving, no polyester yarn was grafted, resulting in reduced flame retardancy. A comparison between Comparative Example 2 and Example 4 shows that in the preparation of the modified polyester yarns suitable for light sizing in water-jet weaving, the polyacrylate-SiO2 nano-hybrid sizing agent was replaced with polyacrylate, leading to reduced flame retardancy. A comparison between Comparative Example 3 and Example 4 shows that in the preparation of the modified polyester yarns suitable for light sizing in water-jet weaving, no corona treatment was performed on the grafted polyester yarn, resulting in reduced uniformity of the sizing agent and fiber bonding, easy peeling of the sizing agent, and reduced flame retardancy.
[0091] The above description is only a preferred embodiment of the present invention, but the scope of protection of the present invention is not limited thereto. Any equivalent substitutions or modifications made by those skilled in the art within the scope of the technology disclosed in the present invention, based on the technical solution and inventive concept of the present invention, should be covered within the scope of protection of the present invention.
[0092] The preferred embodiments of the present invention disclosed above are merely illustrative of the invention. These preferred embodiments do not exhaustively describe all details, nor do they limit the invention to specific implementations. Clearly, many modifications and variations can be made based on the content of this specification. This specification selects and specifically describes these embodiments to better explain the principles and practical applications of the invention, thereby enabling those skilled in the art to better understand and utilize the invention. The invention is limited only by the claims and their full scope and equivalents.
Claims
1. A method for preparing modified polyester yarn suitable for water-jet weaving and light sizing, characterized in that, Includes the following steps: Step (1) Immerse the polyester yarn in an aqueous solution containing DOPO-HEMA and a photoinitiator, heat it, take it out and squeeze it, then irradiate it with ultraviolet light, wash it, and dry it to obtain grafted polyester yarn. Step (2) After corona treatment of the grafted polyester yarn, the nano-hybrid material slurry is used to sizing the grafted polyester yarn to obtain a modified polyester yarn suitable for light sizing in water jet weaving; the nano-hybrid material slurry specifically includes the following components by weight: 35-45 parts of water-soluble polyester, 50-65 parts of polyacrylate-SiO2 nano-hybrid slurry, 0.5-1 parts of penetrant, and 0.8-1.5 parts of antistatic agent.
2. The method for preparing modified polyester yarn suitable for water-jet weaving and light sizing according to claim 1, characterized in that, In step (1), the polyester yarn is a lightly twisted polyester staple fiber yarn with a yarn count of 10s, 16s, or 21s; the bath ratio of the polyester yarn to the aqueous solution is 1:(5-15); the DOPO-HEMA content is 35-45wt%; the photoinitiator is Ir-2959 with a photoinitiator content of 3wt%; the heating conditions are: heating temperature of 55-65℃ and heating time of 1.5-2.5h; the extrusion degree is to extrude to a liquid retention rate of 110-130wt%; the ultraviolet irradiation method is: wrap with cellophane to isolate air, fix it between two glass plates, and irradiate both sides under 365nm ultraviolet light at a distance of 15cm for 8-12min each; the washing method is: wash with distilled water at 75-85℃ for 4-6h. Drying method: Dry at 55-65℃ until constant weight.
3. The method for preparing modified polyester yarn suitable for water-jet weaving and light sizing according to claim 1, characterized in that, The preparation method of DOPO-HEMA in step (1) includes the following steps: DOPO was added to tetrahydrofuran, carbon tetrachloride was added in an ice-water bath, and after the reaction, triethylamine was added, followed by slow dropwise addition of hydroxyethyl methacrylate (HEMA). After the addition was complete, the temperature was raised and stirring was continued until the reaction was stopped. Impurities were removed, the mixture was dried, filtered, and the solvent was evaporated to obtain DOPO-HEMA.
4. The method for preparing modified polyester yarn suitable for water-jet weaving and light sizing according to claim 3, characterized in that, The ratio of DOPO, tetrahydrofuran, carbon tetrachloride, triethylamine, and hydroxyethyl methacrylate is 21.6-30g:200-300mL:110-165mL:13.2-20g:15.6-23.4g; the reaction time is 9-14min; the heating temperature is 35-40℃; the stirring time is 3-6h; the impurity removal method is vacuum filtration, and the filtrate is washed 3-5 times successively with 3% NaOH solution, distilled water, and saturated NaCl aqueous solution; the drying method is to dry the organic layer with anhydrous MgSO4 overnight.
5. The method for preparing modified polyester yarn suitable for water-jet weaving and light sizing according to claim 1, characterized in that, In step (2), the corona treatment conditions are as follows: the corona treatment voltage is 8-10kV and the corona treatment time is 5-10s; the sizing method is as follows: the grafted polyester yarn is immersed in the nano-hybrid material sizing, and sizing is carried out under the conditions of sizing tank temperature of 40-50℃, desizing temperature of 100-105℃, and sizing speed of 30-60m / min; the sizing rate relative to the dry weight of the yarn is 2-4%; the penetrant is JFC; and the antistatic agent is SK-E.
6. The method for preparing modified polyester yarn suitable for water-jet weaving and light sizing according to claim 1, characterized in that, The preparation method of the polyacrylate-SiO2 nano-hybrid slurry in step (2) includes the following steps: S1: Add nano-silica to methanol, heat and stir, then slowly add silane coupling agent, continue stirring, wash, and dry to obtain silanized nano-silica; S2: Diphenylphosphoric acid was dissolved in anhydrous ethanol and stirred to obtain a diphenylphosphoric acid solution; cytosine was dissolved in deionized water and stirred to obtain a cytosine solution; the diphenylphosphoric acid solution and the cytosine solution were mixed and stirred again, then silanized nano-silica was added, the reaction was continued, filtered, and washed to obtain modified nano-SiO2; S3: Modified nano-SiO2 is added to ethanol and ultrasonically treated to obtain nano-SiO2 dispersion. Then, polyacrylate slurry is added, stirred, and ultrasonically treated to obtain polyacrylate-SiO2 nano-hybrid slurry.
7. The method for preparing modified polyester yarn suitable for water-jet weaving and light sizing according to claim 6, characterized in that, In step S1, the ratio of nano-silica, methanol, and silane coupling agent is 50-75g:5-7.5L:10-15mL; the heating and stirring conditions are: heating and stirring temperature is 65-75℃, heating and stirring time is 10-15min; the silane coupling agent is KH-560; the stirring time is continued for 3-5h; the washing method is: washing with methanol and deionized water 3-5 times respectively. In step S2, the ratio of diphenylphosphoric acid, anhydrous ethanol, cytosine, deionized water, and silanized nano-silica is 65.5-98.3g:2-3L:333.3-500g:2-3L:10-15g; the stirring time is 10-20min; the re-stirring time is 5-10min; the conditions for continued stirring are: continued stirring temperature of 65-75℃, continued stirring time of 3-5h; and continued reaction time of 3-5h. In step S3, the ratio of modified nano-SiO2, ethanol, and polyacrylate slurry is 10-15:250-370:210-315; the ultrasonic treatment conditions are: ultrasonic power of 200-300W and ultrasonic treatment time of 15-20min; the stirring treatment conditions are: stirring temperature of 90-100℃ and stirring time of 1-1.5h; and the ultrasonic treatment time is 15-25min.
8. The method for preparing modified polyester yarn suitable for water-jet weaving and light sizing according to claim 7, characterized in that, A method for preparing polyacrylate slurry includes the following steps: Deionized water, sodium dodecylbenzenesulfonate, sodium dodecyl sulfate, methyl acrylate, and butyl acrylate are mixed and stirred to obtain a mixture. Then, acrylic acid, acrylamide, water, and ammonium persulfate are added dropwise to the mixture, and stirring is continued. The mixture is heated, stirred, and kept at the temperature before being cooled. Ammonia water is added dropwise to neutralize the mixture, and the mixture is filtered to obtain a polyacrylate slurry.
9. The method for preparing modified polyester yarn suitable for water-jet weaving and light sizing according to claim 8, characterized in that, The ratio of deionized water, sodium dodecylbenzenesulfonate, sodium dodecyl sulfate, methyl acrylate, butyl acrylate, acrylic acid, acrylamide, water, and ammonium persulfate is 2-4L:20-40g:10-20g:60-120g:530-1060g:260-520g:450-900g:100-200g:40-80g; the stirring conditions are: stirring temperature 55-65℃, stirring time 40-60min; the continued stirring method is: continue stirring at 70-80℃ at a speed of 100-140r / min for 1.5-2.5h; the heating temperature is 82-95℃; the stirring and holding time is 0.5-1.5h; the cooling temperature is 40-50℃; and the ammonia concentration is 28wt%.
10. A modified polyester yarn suitable for light sizing in water-jet weaving, prepared by the method according to any one of claims 1-9.