Polyphenylene sulfide composite material for improving dyeing performance and preparation method thereof
By introducing polyschiff base and modified light-resistant particles into polystyrene sulfide fibers, the problems of poor dyeing performance and degradation of mechanical properties of polystyrene sulfide fibers are solved, and a polystyrene sulfide composite material with high dyeing depth and good stability is achieved.
Patent Information
- Application Number
- CN202510661514.X
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2025-05-22
- Publication Date
- 2025-07-25
AI Technical Summary
The dyeing performance of polyphenylene sulfide fibers is poor, and the crystallinity is high, resulting in impermeability of dye molecules, and the mechanical properties decrease after repeated washing.
Polyschiff base is synthesized using C4-C8 aliphatic dialdehyde, aromatic hydroxy dialdehyde and diaminodiphenyl sulfide, and modified light-resistant particles are prepared by a silane coupling agent modified nanolight shielding agent, which is uniformly dispersed in the polyphenylene sulfide, reducing crystallinity and improving dye binding.
The dyeing depth and fastness of the polyphenylene sulfide composite material are improved, while maintaining good mechanical properties. The mechanical properties of the fibers are decayed less after repeated washing, and have good long-term stability.
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Abstract
Description
Technical Field
[0001] The present invention belongs to the technical field of polyphenylene sulfide fibers, and particularly relates to a polyphenylene sulfide composite material with improved dyeing performance and a preparation method thereof. Background Art
[0002] Polyphenylene sulfide (PPS) fibers are prepared by processes such as melt spinning, hot stretching, and heat setting of linear polyphenylene sulfide. It has a rigid main chain structure with sulfur atoms symmetrically connected to benzene rings at the para position, a relatively high glass transition temperature between 106 - 112 °C, and a crystallinity as high as over 50%, resulting in a low moisture regain, poor wearing comfort, and difficult dyeing, which limits its development and application in clothing.
[0003] Researchers have conducted a large number of explorations to improve the moisture regain and dyeing performance of polyphenylene sulfide fibers. For example, the dyeing process of polyphenylene sulfide fibers disclosed in Patent CN101824759B uses sodium sulfide and p - dichlorobenzene as raw materials, and a solvent system with sulfolane as the solvent to obtain polyphenylene sulfide fibers. After pretreatment by soaking in a 3% - 5% hypochlorite dextrin solution for 5 - 15 min at a treatment temperature of 50 - 53 °C, it is then soaked in an aqueous alcohol solution of 5 - 8% reactive dye for 15 - 60 min, and then dried by hot air to obtain a polyphenylene sulfide fiber dyeing product. It overcomes the problem of difficult dyeing of PPS fibers through the surface pretreatment of the fiber with a hypochlorite dextrin solution and the dyeing with an aqueous alcohol solution of reactive dye. However, the molecular chains in the crystalline region are arranged tightly, and the dye molecules cannot penetrate, but can only adhere to the surface and are easily shed during friction. Patent CN111519273B discloses a moisture - absorbent and easily dyed modified polyphenylene sulfide composite fiber, its preparation method and application. By adding sodium polyacrylate and nano - titanium dioxide to linear polyphenylene sulfide resin, it is extruded into a modified polyphenylene sulfide composite masterbatch, melted into a melt at a temperature of 280 - 320 °C and a pressure of 5 - 10 Mpa, spun through a spinneret, cooled and solidified by annular blowing, and stretched to prepare. It not only solves the problems of difficult dyeing and easy shedding during friction by incorporating sodium polyacrylate internally, but also improves the moisture regain. However, due to the excellent hydrophilicity of sodium polyacrylate, the molecular chain spacing increases (swells) after absorbing water, and repeated washing - drying easily causes micro - cracks or interfacial debonding, resulting in a decrease in the tensile strength of the fiber, that is, the long - term stability of the fiber is not good.
[0004] Therefore, it is urgent to develop a polyphenylene sulfide composite material with good dyeing performance, mechanical properties, and washability. Summary of the Invention
[0005] To solve the above technical problems, the present invention provides a polyphenylene sulfide composite material for improving dyeing performance and its application. A poly-Schiff base containing carbon-nitrogen double bonds and hydroxyl groups that can bind to dyes is prepared from aliphatic dialdehydes, aromatic hydroxyl dialdehydes, and diaminodiphenyl sulfide. The three substances of aliphatic dialdehydes, aromatic hydroxyl dialdehydes, and diaminodiphenyl sulfide cooperate with each other to adjust the polarity of the poly-Schiff base to be close to that of polyphenylene sulfide. The poly-Schiff base can be evenly dispersed in polyphenylene sulfide. At the same time, the rigid chain segments formed by aromatic hydroxyl dialdehydes and diaminodiphenyl sulfide in the poly-Schiff base hinder the close packing of PPS chains, reduce the crystallinity of PPS, and improve the dye uptake rate of the composite material.
[0006] To achieve the above object, the following technical solutions are adopted:
[0007] A polyphenylene sulfide composite material for improving dyeing performance, comprising the following raw materials in parts by weight: 100 parts of linear polyphenylene sulfide, 3-5 parts of poly-Schiff base, and 0.5-0.8 parts of modified lightfast particles; the poly-Schiff base is prepared by a Schiff base reaction of C4-C8 aliphatic dialdehyde, aromatic hydroxyl dialdehyde, and diaminodiphenyl sulfide in a molar ratio of 0.2-0.3:0.6-0.7:1-1.2, wherein the amounts of C4-C8 aliphatic dialdehyde, aromatic hydroxyl dialdehyde, and diaminodiphenyl sulfide satisfy a molar ratio of aldehyde groups to amino groups of 0.8-1:1-1.2; the modified lightfast particles are prepared by surface modification of nano light shielding agents with silane coupling agents, and the nano light shielding agents are selected from one or a combination of two or more of nano zinc oxide, nano titanium dioxide, nano cerium oxide, nano tin antimonate oxide, and nano carbon black.
[0008] The C4-C8 aliphatic dialdehyde is selected from one or a combination of two or more of octanedialdehyde, heptanedialdehyde, hexanedialdehyde, glutaraldehyde, and butanedialdehyde.
[0009] The aromatic hydroxyl dialdehyde is selected from one or a combination of two or more of 2-hydroxyisophthalaldehyde, 4-hydroxyisophthalaldehyde, 5-hydroxyisophthalaldehyde, and 2-hydroxyterephthalaldehyde.
[0010] The diaminodiphenyl sulfide is selected from one or a combination of two of 4,4-diaminodiphenyl sulfide and 2,2'-diaminodiphenyl sulfide.
[0011] After a large number of experiments, the inventor unexpectedly found that when the molar ratio of C4-C8 aliphatic dialdehyde, aromatic hydroxy dialdehyde, and diamino diphenyl sulfide is 0.2-0.3:0.6-0.7:1-1.2, the polyphenylene sulfide composite material can achieve dual optimization of mechanical properties and dyeing properties and reach the best balance state. It is speculated that this molar ratio can make the poly Schiff base and polyphenylene sulfide have good compatibility, will not produce phase separation, and will not affect the mechanical properties. At the same time, it can give full play to the role of the groups and rigid segments that can be combined with the dye on the poly Schiff base, so that the dye molecules can more easily penetrate into the material, and form a stable dyeing structure inside the material, greatly improving the dyeing depth and dyeing fastness. Otherwise, once deviating from this optimal molar ratio range, whether the ratio and content of C4-C8 aliphatic dialdehyde and aromatic hydroxy dialdehyde are too high or too low, or the ratio of diamino diphenyl sulfide is unbalanced, the reaction balance between the raw materials will be broken, and the molecular structure of the poly Schiff base will change. The compatibility between the generated polySchiff base and polyphenylene sulfide will be seriously affected, the phase separation will be aggravated, and a clear phase interface will appear inside the material. This will not only weaken the mechanical properties of the material, but also destroy the effective sites and structures for the polySchiff base to bind to the dye, resulting in a significant reduction in the dyeing performance of the composite material, which cannot meet the needs of practical applications.
[0012] The poly Schiff base is prepared by a method comprising the following steps:
[0013] C4-C8 aliphatic dialdehyde, aromatic hydroxy dialdehyde and diaminodiphenyl sulfide are added to a solvent to dissolve and mix, and the mixture is heated to reflux state under an inert atmosphere to react. After the reaction is completed, a precipitant is added to obtain a poly Schiff base.
[0014] The solvent is selected from one or a combination of two or more of N,N-dimethylformamide, dimethyl sulfoxide, and N,N-dimethylacetamide. The reaction time in the reflux state is 24-48 hours.
[0015] The precipitant is selected from one or a combination of two or more of ether, acetone and methyl ethyl ketone.
[0016] After adding the precipitant, centrifugation, washing and drying are further performed. The washing is performed by washing with alcohol and water alternately for 1-3 times. The drying is performed at a vacuum degree of 0.01-0.1 MPa and 60-100° C. for 1-5 hours.
[0017] The weight average molecular weight of the linear polyphenylene sulfide is 30,000-60,000.
[0018] The modified light-resistant particles are prepared by modifying the surface of a nano light-shielding agent with a silane coupling agent.
[0019] Further, the modified light-resistant particles are prepared by a method including the following steps: adding a nano light-shielding agent into a preheated silane coupling agent dispersion liquid, heating to the reflux state for reaction, and filtering, washing, and drying after the reaction to obtain the modified light-resistant particles.
[0020] The preheating temperature is 60 - 80°C. The mass-volume ratio of the nano light-shielding agent to the silane coupling agent solution is 1:5 - 10 (g / ml). The concentration of the silane coupling agent in the silane coupling agent dispersion liquid is 5 - 8 wt%. The solvent of the silane coupling agent solution is selected from one or a combination of two of toluene and benzene. The reaction time is 12 - 24 h.
[0021] The silane coupling agent is selected from one or a combination of two or more of an amino silane coupling agent, an epoxy silane coupling agent, a phenyl silane coupling agent, and a fluorinated silane coupling agent, and preferably a fluorinated silane coupling agent.
[0022] The fluorinated silane coupling agent is selected from one or a combination of two or more of tridecafluorooctyltrimethoxysilane, heptadecafluorodecyltripropoxysilane, per(heptadeca)fluorodecyltrimethoxysilane, nonafluorohexyltrimethoxysilane, triethoxy-1H,1H,2H,2H-perfluorodecylsilane, tridecafluorooctyltrimethoxysilane, 3,3,3-trifluoropropyltriethoxysilane, and 3,3,3-trifluoropropylmethyldimethoxysilane, and preferably tridecafluorooctyltrimethoxysilane.
[0023] The average particle size of the nano light-shielding agent is 30 - 60 nm.
[0024] The inventors found that when the silane coupling agent is a fluorinated silane coupling agent, it can not only ensure the uniform dispersion of the modified light-resistant particles in the polyphenylene sulfide composite material, but also improve the dye uptake rate of the polyphenylene sulfide composite fiber. It is speculated that the fluorinated silane coupling agent on the surface of the modified light-resistant particles will make their distribution in the composite material system more uniform, and at the same time will also hinder the adsorption and regular arrangement of the polyphenylene sulfide molecular chain on the surface of the modified light-resistant particles, thereby inhibiting the formation and growth of crystal nuclei, reducing the crystallinity of polyphenylene sulfide, and improving the dyeing performance.
[0025] The present invention also provides a preparation method of the polyphenylene sulfide composite material with improved dyeing performance, including the following steps:
[0026] Mixing linear polyphenylene sulfide, poly Schiff base, and modified light-resistant particles, and performing extrusion granulation to obtain the polyphenylene sulfide composite material with improved dyeing performance.
[0027] The extrusion granulation is carried out by using a twin-screw extruder. The temperature of the first zone of the screw is 260 - 280°C, the temperature of the second zone of the screw is 280 - 300°C, the temperature of the third zone of the screw is 300 - 310°C, the temperature of the discharge die orifice is 305 - 310°C, and the screw speed is 150 - 200 rpm.
[0028] The present invention also provides an application of a polyphenylene sulfide composite material with improved dyeing performance, and the polyphenylene sulfide composite material with improved dyeing performance is used for preparing polyphenylene sulfide composite fibers with improved dyeing performance.
[0029] The application includes the following steps: melt-spinning, drawing, stretching, heat setting, crimping, and cutting the above-mentioned polyphenylene sulfide composite material with improved dyeing performance to obtain polyphenylene sulfide composite fibers with improved dyeing performance.
[0030] The temperatures of the first, second, third, and fourth zones of the melt spinning are 260 - 280 °C, 280 - 320 °C, 320 - 330 °C, and 330 - 335 °C respectively. The pore diameter of the spinneret holes of the spinneret plate is 0.1 - 1.0 mm, and the ratio of the length to the diameter of the spinneret holes is 2.0 - 10.0. The drawing speed is 500 - 1000 m / min. The stretching temperature is 60 - 100 °C, and the stretching multiple is 2 - 8 times. The heat setting temperature is 100 - 160 °C. The winding speed is 500 - 2000 m / min.
[0031] Compared with the prior art, the beneficial effects of the present invention are:
[0032] First, the present invention uses C4 - C8 aliphatic dialdehydes, aromatic hydroxy dialdehydes, and diaminodiphenyl sulfide as raw materials to prepare poly Schiff bases containing carbon-nitrogen double bonds and hydroxyl groups that can bind to dyes in the molecular chain. The three substances of C4 - C8 aliphatic dialdehydes, aromatic hydroxy dialdehydes, and diaminodiphenyl sulfide cooperate with each other to adjust the polarity of the poly Schiff base to be close to that of polyphenylene sulfide. The poly Schiff base can be uniformly dispersed in polyphenylene sulfide. At the same time, the rigid chain segments formed by aromatic hydroxy dialdehydes and diaminodiphenyl sulfide in the poly Schiff base hinder the close packing of PPS chains, reduce the crystallinity of PPS, and improve the dye uptake rate of the composite material.
[0033] Second, the inventors found that when the silane coupling agent is a fluorine-containing silane coupling agent, it can not only ensure the uniform dispersion of the modified light-resistant particles in the polyphenylene sulfide composite material, but also improve the dye uptake rate of the polyphenylene sulfide composite fiber. At this time, the fiber has good mechanical properties and dyeing performance.
[0034] Third, the polyphenylene sulfide composite fiber prepared by the present invention has a small decrease in mechanical properties after repeated washing and drying, and the fiber has good long-term stability. The fabric prepared from this fiber is strong and wash-resistant. Specific Embodiments
[0035] The following further illustrates the present invention in combination with specific embodiments, but is not limited to the content in the specification. Unless otherwise specified, the "parts" mentioned in the embodiments of the present invention are all parts by weight. The reagents used are all commercially available reagents in the art.
[0036] The rutile-type nano-titanium dioxide was purchased from Hangzhou Wanjing New Materials Co., Ltd., and the average particle size of VK-T25 was 30 nm.
[0037] Linear polyphenylene sulfide was purchased from Jiangxi Juzhen Technology Development Co., Ltd., and the weight-average molecular weight was 57,000 g / mol.
[0038] Example 1
[0039] 1) 3 mol of succinaldehyde, 7 mol of 2-hydroxyisophthalaldehyde, and 12 mol of 4,4-diaminodiphenyl sulfide were added to 10 L of N,N-dimethylacetamide for dissolution and mixing. Under a nitrogen atmosphere, the temperature was raised to the reflux state and reacted for 24 h. After the reaction, methyl ethyl ketone was added until no precipitation occurred, followed by centrifugation. It was washed 3 times alternately with water and ethanol, and dried at a vacuum degree of 0.08 MPa and 60 °C for 1.5 h to obtain poly-Schiff base.
[0040] 2) The rutile-type nano-titanium dioxide VK-T25 was added to a dispersion liquid (with toluene as the solvent) with a concentration of 8 wt% of tridecafluorooctyltrimethoxysilane at 80 °C at a mass-to-volume ratio of 1:10 (g / ml). The temperature was raised to the reflux state and reacted for 24 h. After the reaction, it was filtered, washed 3 times alternately with ethanol and water, and dried at 80 °C to constant weight to obtain modified light-resistant particles.
[0041] 3) 100 parts by mass of linear polyphenylene sulfide, 5 parts by mass of poly-Schiff base, and 0.8 parts by mass of modified light-resistant particles were added to a high-speed mixer for mixing, and then added to a twin-screw extruder for extrusion granulation to obtain a polyphenylene sulfide composite material with improved dyeing performance. The temperature of the first zone of the screw was 280 °C, the temperature of the second zone of the screw was 300 °C, the temperature of the third zone of the screw was 310 °C, the temperature of the die orifice was 310 °C, and the screw speed was 200 rpm.
[0042] 4) The polyphenylene sulfide composite material with improved dyeing performance was added to a single-screw melt spinning machine. The temperatures of the first, second, third, and fourth zones for melt spinning were 280 °C, 300 °C, 320 °C, and 330 °C respectively. The pore diameter of the spinneret holes of the spinneret plate was 0.35 mm, and the ratio of the length to the diameter of the spinneret holes was 4. The spinning oil POY-2048 was applied, and it was drawn at a speed of 600 m / min, stretched at a temperature of 100 °C with a stretching ratio of 2.5 times, heat-set at a temperature of 160 °C, and crimped and cut at a speed of 2000 m / min to obtain polyphenylene sulfide composite fibers with a linear density of 74.3 dtex / 18f and improved dyeing performance.
[0043] Example 2
[0044] The rest was the same as in Example 1, except that in step 1), the amount of 4,4-diaminodiphenyl sulfide used was 10 mol.
[0045] Example 3
[0046] The rest is the same as in Example 1, except that in step 1), the amount of 2-hydroxyisophthalaldehyde used is 6 mol.
[0047] Example 4
[0048] The rest is the same as in Example 1, except that in step 1), the amount of succinaldehyde used is 2 mol.
[0049] Example 5
[0050] The rest is the same as in Example 1, except that in step 1), succinaldehyde is replaced with an equimolar amount of octanedial.
[0051] Example 6
[0052] The rest is the same as in Example 1, except that in step 1), 2-hydroxyisophthalaldehyde is replaced with an equimolar amount of 2-hydroxypterophthalaldehyde.
[0053] Example 7
[0054] The rest is the same as in Example 1, except that in step 3), the amount of the poly Schiff base used is 3 parts by mass.
[0055] Example 8
[0056] The rest is the same as in Example 1, except that in step 2), 3-aminopropyltrimethoxysilane is used to replace tridecafluorooctyltrimethoxysilane in an equal mass.
[0057] Example 9
[0058] 1) Add 2 mol of succinaldehyde, 7 mol of 2-hydroxyisophthalaldehyde, and 12 mol of 4,4'-diaminodiphenyl sulfide to 10 L of N,N-dimethylacetamide, dissolve and mix well. Under a nitrogen atmosphere, heat to the reflux state and react for 24 h. After the reaction is completed, add methyl ethyl ketone until no precipitate is produced, centrifuge, wash alternately with water and ethanol 3 times, and dry at a vacuum degree of 0.08 MPa and 60 °C for 1.5 h to obtain the poly Schiff base.
[0059] 2) Add rutile-type nano-titanium dioxide VK-T25 according to a mass-to-volume ratio of 1:5 (g / ml) to a dispersion liquid (solvent is toluene) with a concentration of 8 wt% of tridecafluorooctyltrimethoxysilane at 80 °C, heat to the reflux state and react for 24 h. After the reaction is completed, filter, wash alternately with ethanol and water 3 times, and dry at 80 °C to constant weight to obtain the modified light-resistant particles.
[0060] 3) Mix 100 parts by mass of linear polyphenylene sulfide, 3 parts by mass of poly Schiff base, and 0.5 part by mass of modified light-fast particles in a high-speed mixer, and add the mixture to a twin-screw extruder for extrusion granulation to obtain a polyphenylene sulfide composite material with improved dyeing performance. The temperature of the first zone of the screw is 280 °C, the temperature of the second zone of the screw is 300 °C, the temperature of the third zone of the screw is 310 °C, the temperature of the discharge die orifice is 310 °C, and the screw speed is 200 rpm.
[0061] 4) Add the polyphenylene sulfide composite material with improved dyeing performance to a single-screw melt spinning machine. The temperatures of the first, second, third, and fourth zones for melt spinning are 280 °C, 300 °C, 320 °C, and 330 °C respectively. The aperture diameter of the spinneret holes of the spinneret plate is 0.35 mm, and the ratio of the length to the diameter of the spinneret holes is 4. Spin finish POY-2048 is applied. The material is drawn at a speed of 600 m / min, stretched at a temperature of 100 °C with a stretching ratio of 2.5 times, heat-set at a temperature of 160 °C, crimped at a speed of 2000 m / min, and cut to obtain polyphenylene sulfide composite fibers with improved dyeing performance.
[0062] Comparative Example 1
[0063] The rest is the same as in Example 1, except that in step 1), the amount of succinaldehyde used is 4 mol and the amount of 2-hydroxyisophthalaldehyde used is 6 mol.
[0064] Comparative Example 2
[0065] The rest is the same as in Example 1, except that in step 1), the amount of succinaldehyde used is 2 mol and the amount of 2-hydroxyisophthalaldehyde used is 8 mol.
[0066] Comparative Example 3
[0067] Refer to the formulation in Example 1 of Patent CN111519273B for granulation and spinning to prepare polyphenylene sulfide composite fibers:
[0068] 1) Mix 100 parts by mass of linear polyphenylene sulfide, 1 part by mass of sodium polyacrylate (purchased from Shanghai Lianmai Biotech Co., Ltd., product number JH-08, weight-average molecular weight 30 million, average particle size 61 μm), and 1 part by mass of rutile-type nano titanium dioxide VK-T25 in a high-speed mixer, and add the mixture to a twin-screw extruder for extrusion granulation to obtain a polyphenylene sulfide composite material with improved dyeing performance. The temperature of the first zone of the screw is 280 °C, the temperature of the second zone of the screw is 300 °C, the temperature of the third zone of the screw is 310 °C, the temperature of the discharge die orifice is 310 °C, and the screw speed is 200 rpm.
[0069] 2) Add the polyphenylene sulfide composite material with improved dyeing performance to a single-screw melt spinning agent. The temperatures of the first, second, third, and fourth zones of melt spinning are 280 °C, 300 °C, 320 °C, and 330 °C respectively. The pore diameter of the spinneret holes is 0.35 mm, and the ratio of the hole length to the diameter is 4. Apply the spinning oil POY-2048, draw at a speed of 600 m / min, stretch at a temperature of 100 °C with a stretching ratio of 2.5 times, perform heat setting at a temperature of 160 °C, curl at a speed of 2000 m / min, and cut to obtain polyphenylene sulfide composite fibers.
[0070] Application examples and comparative application examples
[0071] Preparation of cleaning solution: 2 g / L of sodium hydroxide, 2 g / L of soap flakes, and the rest is water.
[0072] Cleaning: Immerse the polyphenylene sulfide composite fibers obtained in Examples 1-9 or Comparative Examples 1-2 in the cleaning solution at a bath ratio of 1:100 (g / ml), heat to 90 °C and treat for 40 min, then rinse with hot water at 60 °C for 10 min, rinse with normal temperature water, and finally dry in an oven at 90 °C for 20 min.
[0073] Preparation of dyeing solution: Add 2% disperse blue 2BLN (Zhejiang Longsheng Group Co., Ltd.), 1.0% ethylene glycol monomethyl ether leveling agent, and 2% sodium dodecyl sulfonate dispersant, and adjust the pH of the dyeing solution to 4.0 with an acetic acid-sodium acetate buffer solution with a pH of 3.
[0074] Dyeing process: Immerse the PPS fabric to be dyed in the prepared dyeing solution according to a bath ratio of 1:20, enter the dye bath at room temperature, raise the temperature to 80 °C at 4 °C / min, then raise the temperature to 130 °C at 1 °C / min, keep the temperature at 130 °C for 30 min, then cool down to room temperature, take out, wash twice with water at 70 °C, and dry in an oven at 80 °C for 20 minutes.
[0075] Reductive cleaning: Immerse the polyphenylene sulfide composite fibers in the reductive cleaning solution at 80 °C according to a bath ratio of 1:30. The concentration of sodium hydroxide in the reductive cleaning solution is 2 g / L and the concentration of sodium dithionite is 3 g / L. Perform reductive cleaning in the reductive cleaning solution for 30 min, wash twice with hot water at 80 °C and twice with cold water in sequence, and then dry in an oven at 80 °C for 20 minutes.
[0076] Perform the following performance tests on the fibers prepared in the above application examples and comparative application examples:
[0077] Tensile strength: Refer to the test method for the tensile properties of chemical fiber filaments GB / T 14344-2008. After the fibers are balanced at 20 °C and a relative humidity of 65% for 24 h, perform the test. The length of the fiber specimen held is 250 mm, and the stretching is carried out at 150 mm / min. Repeat the test 10 times and take the average value.
[0078] Dye uptake: calculated by measuring the ratio of the absorbance of the residual liquid after dyeing to the absorbance of the original dye solution. The test uses a TU-1900 double-beam UV-visible spectrophotometer to measure the absorbance A0 and Ai of the dye solution before and after dyeing. The dye uptake E is calculated according to the following formula:
[0079] E=(1-A i / A0)*100%
[0080] Color fastness to washing with soap: refer to GB / T 3921-2008 Textile color fastness test for color fastness to washing with soap for testing. Take the fiber and sandwich it between two 100mm*40mm single fiber adjacent fabrics, one is cotton fiber adjacent fabric, and the other is wool adjacent fabric. Add soap solution, raise its temperature to 50±2℃, and the bath ratio is 50:1. Cover the container and wash for 45 minutes by rinsing under the condition of keeping the solution temperature at 50±2℃. After washing, wash the sample twice with three-level water and dry it at 40℃. Use the gray sample card (GB / T251-1995) to compare with the original sample to evaluate the fading fastness.
[0081] Washability test: immerse the tensile strength specimen in water with a bath ratio of 50:1, maintain the solution at a constant temperature of 50±2℃ for 30 minutes, and then dry it at 40℃. This is one cycle. After 100 cycles, re-measure the above tensile strength and calculate the tensile strength loss rate.
[0082] Table 1 Performance test results
[0083]
[0084]
[0085] It can be seen from Table 1 that the polyphenylene sulfide composite fiber prepared by the present invention has high dye uptake, high soap fastness, excellent mechanical properties, little attenuation of mechanical properties after repeated washing and drying, and good long-term fiber stability.
[0086] The above detailed description is a specific description of one feasible embodiment of the present invention. The embodiment is not intended to limit the patent scope of the present invention. Any equivalent implementation or modification that does not deviate from the present invention should be included in the scope of the technical solution of the present invention.
Claims
1. A polyphenylene sulfide composite material for improving dyeing performance, characterized in that, It comprises raw materials in the following parts by weight: 100 parts of linear polyphenylene sulfide, 3 - 5 parts of poly Schiff base, and 0.5 - 0.8 part of modified lightfast particles; the poly Schiff base is prepared by a Schiff base reaction of C4 - C8 aliphatic dialdehyde, aromatic hydroxyl dialdehyde, and diaminodiphenyl sulfide in a molar ratio of 0.2 - 0.3:0.6 - 0.7:1 - 1.2, wherein the amounts of C4 - C8 aliphatic dialdehyde, aromatic hydroxyl dialdehyde, and diaminodiphenyl sulfide satisfy a molar ratio of aldehyde group to amino group of 0.8 - 1:1 - 1.2; the modified lightfast particles are prepared by surface modification of nano light shielding agent with silane coupling agent, and the nano light shielding agent is selected from one or a combination of two or more of nano zinc oxide, nano titanium dioxide, nano cerium oxide, nano antimony tin oxide, and nano carbon black.
2. The polyphenylene sulfide composite material for improving dyeing performance according to claim 1, wherein The C4 - C8 aliphatic dialdehyde is selected from one or a combination of two or more of octanedial, heptanedial, hexanedial, pentanedial, and butanedial; the aromatic hydroxyl dialdehyde is selected from one or a combination of two or more of 2 - hydroxyisophthalaldehyde, 4 - hydroxyisophthalaldehyde, 5 - hydroxyisophthalaldehyde, and 2 - hydroxyterephthalaldehyde; the diaminodiphenyl sulfide is selected from one or a combination of two of 4,4 - diaminodiphenyl sulfide and 2,2'-diaminodiphenyl sulfide.
3. The polyphenylene sulfide composite material for improving dyeing performance according to claim 1, wherein The poly Schiff base is prepared by a method comprising the following steps: Add C4 - C8 aliphatic dialdehyde, aromatic hydroxyl dialdehyde, and diaminodiphenyl sulfide to a solvent for dissolution and mixing, and under an inert atmosphere, heat to the reflux state for reaction. After the reaction is completed, add a precipitating agent to obtain the poly Schiff base.
4. The polyphenylene sulfide composite material for improving dyeing performance according to claim 1, characterized in that, The weight - average molecular weight of the linear polyphenylene sulfide is 30,000 - 60,000; and / or the average particle size of the nano light shielding agent is 30 - 60 nm.
5. The polyphenylene sulfide composite material for improving dyeing performance according to claim 1, wherein, The modified lightfast particles are prepared by a method comprising the following steps: Add the nano light shielding agent to a pre - heated silane coupling agent dispersion liquid, heat to the reflux state for reaction, and after the reaction is completed, filter, wash, and dry to obtain the modified lightfast particles.
6. The polyphenylene sulfide composite material for improving dyeing performance according to claim 1, wherein The silane coupling agent is selected from one or a combination of two or more of amino silane coupling agent, epoxy silane coupling agent, phenyl silane coupling agent, and fluorinated silane coupling agent, and preferably a fluorinated silane coupling agent.
7. The polyphenylene sulfide composite material for improving dyeing performance according to claim 6, wherein The fluorinated silane coupling agent is selected from one or a combination of two or more of tridecafluorooctyltrimethoxysilane, heptadecafluorodecyltripropoxysilane, per(heptadeca)fluorodecyltrimethoxysilane, nonafluorohexyltrimethoxysilane, triethoxy - 1H,1H,2H,2H - perfluorodecylsilane, tridecafluorooctyltrimethoxysilane, 3,3,3 - trifluoropropyltriethoxysilane, and 3,3,3 - trifluoropropylmethyldimethoxysilane, and preferably tridecafluorooctyltrimethoxysilane.
8. The preparation method of the polyphenylene sulfide composite material with improved dyeing performance according to any one of claims 1-7, characterized in that, It comprises the following steps: Mix the linear polyphenylene sulfide, poly Schiff base, and modified lightfast particles, and carry out extrusion granulation to obtain the polyphenylene sulfide composite material with improved dyeing performance.
9. A polyphenylene sulfide composite fiber with improved dyeing performance, which is prepared from the polyphenylene sulfide composite material according to any one of claims 1 - 7.
10. The polyphenylene sulfide composite fiber with improved dyeing performance according to claim 9, wherein, The preparation method of the composite fiber comprises the following steps: performing melt spinning, drawing, stretching, heat setting, crimping, and cutting on the polyphenylene sulfide composite material according to any one of claims 1-7 to obtain the polyphenylene sulfide composite fiber with improved dyeing performance.
Citation Information
Patent Citations
Dyeing process of polyphenylene sulfide fiber
CN101824759B
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