High-fastness high-washability water-absorbing quick-drying resin and application thereof
Through the use of low-branching block polyester polyether hydrophilic resin, the problem of color fastness reduction in polyester fabrics during high-temperature thermal setting is solved, and the high washing resistance and water absorption speed drying performance is improved, and the Good anti-static and easy decontamination effect.
Patent Information
- Application Number
- CN202411430620.9
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2024-10-14
- Publication Date
- 2024-12-13
AI Technical Summary
In the prior art, polyester fabrics cause the color fastness of dyed fabrics to decrease during the high-temperature thermal setting process, and the commercially available hydrophilic quick-drying finishing agents are unstable in the thermal environment, which affects the problem of dye migration, making it difficult to meet the high washing-resistant and water absorption. The requirement for quick-drying performance.
Low-branching block polyester polyether hydrophilic resin is prepared through specific monomer structures and catalytic conditions to form a resin with high viscosity and good emulsification properties, which is used for post-organization of fibers to avoid dye migration and Improves the color fastness and wash resistance of fabrics.
It effectively improves the color fastness and wash resistance of polyester fabrics, avoids dye migration, meets the needs of high washing-resistant, water-absorbing and quick-drying performance, and has good anti-static and easy-to-dirty effects.
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Abstract
Description
Technical Field
[0001] The invention relates to a resin, in particular to a high-fastness, high-washing-resistant, water-absorbing and quick-drying resin and application thereof, belonging to the field of functional finishing of textile fabrics. Background Art
[0002] During the high-temperature heat setting process, disperse dyes will inevitably migrate from the inside of the fiber to the surface due to the thermal activity of the polyester fiber macromolecules and the weakening of the interaction between the dye molecules and the fiber molecules under high heat, resulting in a decrease in the color fastness of the dyed fabric. This is the inherent physical property of disperse dyes on polyester fibers. Padding is a common finishing process in the continuous processing of functional fabrics in printing and dyeing enterprises. The high heat applied to the dyed fabric in this process often causes the color fastness of the fabric to decrease, causing the risk of defective finished products. However, due to the low energy consumption, short time consumption and low finishing cost of the padding finishing process, it is still the best process for printing and dyeing enterprises to complete conventional finishing orders. In addition, the fabrics treated with quick-drying by the padding process generally have a barely qualified quick-drying performance after 5 washes, and often fail to meet the quick-drying performance after 10 washes. With the launch of the updated water absorption and quick-drying standard GB / T 21655.1-2023 in 2023, the demand for quick-drying agents with higher washing durability is also gradually increasing.
[0003] Polyester fabrics have low moisture regain and poor antistatic properties, and hydrophilic quick-drying finishing has almost become an essential processing step for polyester fabrics for daily wear. Most commercially available hydrophilic quick-drying finishing agents are hydrophilic polysiloxanes and linear polyester polyether hydrophilic resins, which will form a layer of "auxiliary film" on the fabric surface after padding. This layer of film acts as a "second phase solvent" to help dissolve disperse dyes that migrate to the fiber surface during padding; if the interaction between the film and the fabric is weak and the strength is poor, it is not enough to limit the migration of dyes, which will further aggravate the decline in the color fastness of the finished fabric. Therefore, the invention of a water-absorbing quick-drying finishing auxiliary with excellent performance and little effect on the color fastness of dyed fabrics, especially a water-absorbing quick-drying finishing auxiliary that can achieve high wash resistance and quick-drying effect, has broad market prospects and practical significance. Summary of the invention
[0004] The present invention mainly solves the deficiencies in the prior art and provides a high-fastness, high-washing-resistant, water-absorbing, quick-drying resin and its application, which has better performance, better color fastness, smaller color change, good durable antistatic effect and easy decontamination.
[0005] The above technical problems of the present invention are mainly solved by the following technical solutions:
[0006] A high fastness, high washability, water-absorbing and quick-drying resin:
[0007] The resin is a low-branched block polyester polyether hydrophilic resin containing a multifunctional small molecular monomer structure, and the structure is as follows:
[0008]
[0009] Wherein, m, n, a, b, c are all natural numbers, 1≤m≤150, 1≤n≤4, 1≤a+b+c≤30; X is a monomer structure with a functionality ≥3;
[0010] Preferably, the molar ratio of the multifunctional small molecule monomer in the low-branching block polyester polyether hydrophilic resin to the total molar ratio of the monomer is 0.1%-40%.
[0011] Preferably, the molar ratio of the total monomers is 0.5-20%.
[0012] Preferably, the multifunctional monomer is a small molecule monomer, and the functional groups in the monomer include one or more of hydroxyl, carboxyl and amino.
[0013] Preferably, the multifunctional small molecule monomer is a polyol or a polycarboxylic acid or a triamine or a mixed monomer thereof.
[0014] Preferably, the multifunctional small molecule monomer is a mixture of one or more of glycerol, triethanolamine, pentaerythritol and trimethylolpropane, dimethylolpropionic acid, dimethylolbutyric acid, pyromellitic anhydride and citric acid.
[0015] Preferably, the low-branching block polyester polyether hydrophilic resin has a melt viscosity of 3000-60000 mPa·s.
[0016] The test conditions are: cone and plate viscometer, 6# rotor, 150°C, 100rpm.
[0017] Preferably, the solvent is one or more of 1,3-dimethyl-2-imidazolidinone, tetramethyl urea, diethylene glycol monobutyl ether, ethylene glycol butyl ether acetate, diethylene glycol and 2-methyl-2,4-pentanediol.
[0018] A method for preparing a high-fastness, high-washing-resistant, water-absorbing and quick-drying resin is carried out according to the following steps:
[0019] (I) Preparation of low-branching block polyester polyether hydrophilic resin:
[0020] Put the polyether diol into a reaction kettle, add ethylene terephthalate, ethylene isophthalate and / or sodium 1,3-dimethyl phthalate-5-sulfonate and a multifunctional small molecule monomer after the polyether diol is completely melted, melt the polyether diol in a N2 atmosphere, and stir and heat up;
[0021] When the temperature rises to 160-180°C, add the catalyst dissolved by ethylene glycol, continue to heat to 200-230°C, and keep warm for 1-3 hours;
[0022] Continue to raise the temperature to 240-260°C, gradually evacuate to below 30 Torr, and keep the temperature and pressure under this condition for polycondensation reaction for 1-5.5 hours. After the reaction is completed, introduce N2 to restore the pressure to normal pressure to obtain a low-branching block polyester polyether hydrophilic resin.
[0023] Preferably, the molar feed ratio of ethylene terephthalate to ethylene isophthalate and / or sodium dimethyl 5-sulfonate is 10:1-1:1;
[0024] The molar feed ratio of ethylene terephthalate to polyether diol is 10:1-2:1;
[0025] The polyether diol is one of polyethylene glycol, polypropylene glycol and polytetrahydrofuran or a mixture thereof, and has a molecular weight range of 600-6000;
[0026] Preferably, the molar feed ratio of ethylene terephthalate to ethylene isophthalate and / or sodium dimethyl 5-sulfonate is 2:1-6:1;
[0027] The molar feed ratio of ethylene terephthalate to polyether diol is 6:1-3:1;
[0028] The molecular weight of polyethylene glycol is 2000-5000, the molecular weight of polypropylene glycol is 3000-5000, and the molecular weight of polytetrahydrofuran is 1000-3000;
[0029] A high-fastness, high-washing-resistant, water-absorbing and quick-drying resin and its application: by post-finishing fabrics, a fiber product containing a low-branching block polyester polyether hydrophilic resin component content of 0.01-10% owf is obtained.
[0030] Preferably, the finishing method includes but is not limited to dyeing in one bath, dyeing in bath and dyeing padding and setting treatment;
[0031] The fabric is mainly PET fabric or a fabric prepared by any spinning and weaving process using PET fiber and other fibers and is subjected to water absorption and quick-drying finishing.
[0032] The present invention relates to a high-fastness, high-washing-resistant, water-absorbing and quick-drying resin and its application, which has the following beneficial effects compared with the prior art:
[0033] 1. The washable water-absorbing quick-drying finishing agent of the present invention has a low-branching polyester polyether hydrophilic resin as the main component. In addition to ensuring excellent washable and quick-drying performance, its good molecular planarity and high film-forming strength can effectively prevent the further migration of disperse dyes on the dyed polyester fabric and ensure the color fastness of the finished fabric. The water-absorbing quick-drying finishing agent of the present invention not only effectively improves the current situation of generally poor color fastness of padding and quick-drying finished polyester dyed fabrics in the industry, but also further improves the washable and quick-drying performance of padding and finishing fabrics on this basis.
[0034] 2. The present invention preferably uses a solvent system with poor alcoholysis performance. On the one hand, the addition of a suitable organic solvent can improve the emulsification performance of the functional resin during the productization process; on the other hand, it can prevent the functional resin from being excessively alcoholyzed in a hot environment, causing serious macromolecular chain scission and affecting the performance of the final product emulsion.
[0035] 3. The resin involved in the present invention has good wash-resistant antistatic effect and easy decontamination effect. DETAILED DESCRIPTION
[0036] The technical solution of the present invention is further specifically described below through embodiments.
[0037] In the following description, a large number of specific details are provided to provide a more thorough understanding of the present invention. However, it is apparent to those skilled in the art that the present invention can be implemented without one or more of these details. In other examples, in order to avoid confusion with the present invention, some technical features well known in the art are not described.
[0038] The present invention will be further described below in conjunction with the embodiments, and the examples of the embodiments are intended to explain the present invention and should not be construed as limiting the present invention. Where specific techniques and reaction conditions are not specified in the embodiments, the techniques or conditions described in the literature in the art or the product specifications may be used.
[0039] Embodiment 1:
[0040] 1) 0.15 mol of PEG-3000 is added to a reaction kettle evacuated with N2 and equipped with a thermometer, a condensing device and a mechanical stirrer. After the reaction kettle is completely melted, 0.68 mol of ethylene terephthalate, 0.01 mol of glycerol and 0.17 mol of ethylene isophthalate are added and the mixture is heated to melt. When the temperature in the kettle rises to 180 (± 2) °C, a composite catalyst of zinc acetate and n-butyl titanate dissolved in 0.9 mol of ethylene glycol is added, the temperature is raised to 230 (± 5) °C, and the reaction is carried out at the maintained temperature to ensure that the distillate amount of the fraction is greater than 95% of the theoretical amount.
[0041] After the temperature was further raised to 250 (± 2) °C, the introduction of N2 was stopped, and the vacuum was slowly evacuated to 5 Torr. Under this condition, the temperature and pressure were maintained to react until the resin viscosity reached 20000 (± 500) mPa.s, thereby obtaining a hydrophilic resin 1.
[0042] 2) N2 was introduced, the temperature was cooled to 160°C with stirring, 3% (mass fraction of the emulsion) of 1,3-dimethyl-2-imidazolidinone was added, the mixture was stirred fully, and the temperature was controlled to 130°C. The mixture was stirred for 1 hour at the temperature, and then the mixture was slowly discharged into an emulsifying kettle pre-filled with 70°C hot water and stirred and dispersed to complete the emulsification of the synthetic resin, thereby obtaining a washable water-absorbing quick-drying agent 1. The application effect is shown in Table 1.
[0043] Embodiment 2:
[0044] 1) 0.15 mol of PEG-3000 is added to a reaction kettle evacuated with N2 and equipped with a thermometer, a condensing device and a mechanical stirrer. After the reaction kettle is completely melted, 0.68 mol of ethylene terephthalate, 0.01 mol of trimethylolpropane and 0.17 mol of ethylene isophthalate are added and the mixture is heated to melt. When the temperature in the kettle rises to 180 (± 2) °C, a composite catalyst of zinc acetate and n-butyl titanate dissolved in 0.9 mol of ethylene glycol is added, the temperature is raised to 230 (± 5) °C, and the reaction is carried out at the maintained temperature to ensure that the distillate amount of the fraction is greater than 95% of the theoretical amount.
[0045] After the temperature was further raised to 250 (± 2) °C, the introduction of N2 was stopped, and the vacuum was slowly evacuated to 5 Torr. Under this condition, the temperature and pressure were maintained to react until the resin viscosity reached 20000 (± 500) mPa.s, thereby obtaining a hydrophilic resin 2.
[0046] 2) N2 was introduced, the temperature was cooled to 160°C with stirring, 3% (mass fraction of the emulsion) of 1,3-dimethyl-2-imidazolidinone was added, the mixture was stirred fully, and the temperature was controlled to 130°C. The mixture was stirred for 1 hour at the temperature, and then the mixture was slowly discharged into an emulsifying kettle pre-filled with 70°C hot water and stirred and dispersed to complete the emulsification of the synthetic resin, thereby obtaining a washable water-absorbing quick-drying agent 2. The application effect is shown in Table 1.
[0047] Embodiment 3:
[0048] 1) 0.15 mol of PEG-4000 is added to a reaction kettle evacuated with N2 and equipped with a thermometer, a condensing device and a mechanical stirrer. After the reaction kettle is completely melted, 0.68 mol of ethylene terephthalate, 0.01 mol of glycerol and 0.17 mol of ethylene isophthalate are added and the mixture is heated to melt. When the temperature in the kettle rises to 180 (± 2) °C, a composite catalyst of zinc acetate and n-butyl titanate dissolved in 0.9 mol of ethylene glycol is added, the temperature is raised to 230 (± 5) °C, and the reaction is carried out at the maintained temperature to ensure that the distillate amount of the fraction is greater than 95% of the theoretical amount.
[0049] After the temperature was further raised to 250 (± 2) °C, the introduction of N2 was stopped, and the vacuum was slowly evacuated to 5 Torr. Under this condition, the temperature and pressure were maintained to react until the resin viscosity reached 20000 (± 500) mPa.s, thereby obtaining hydrophilic resin 3.
[0050] 2) N2 was introduced, the temperature was cooled to 160°C with stirring, 3% (mass fraction of the emulsion) of 1,3-dimethyl-2-imidazolidinone was added, the mixture was stirred fully, and the temperature was controlled to 130°C. The mixture was stirred for 1 hour at the temperature, and then the mixture was slowly discharged into an emulsifying kettle pre-filled with 70°C hot water and stirred and dispersed to complete the emulsification of the synthetic resin, thereby obtaining a washable water-absorbing quick-drying agent 3, the application effect of which is shown in Table 1.
[0051] Embodiment 4:
[0052] 1) 0.15 mol of PEG-6000 is added to a reaction kettle evacuated with N2 and equipped with a thermometer, a condensing device and a mechanical stirrer. After the reaction kettle is completely melted, 0.68 mol of ethylene terephthalate, 0.01 mol of glycerol and 0.17 mol of ethylene isophthalate are added and the mixture is heated to melt. When the temperature in the kettle rises to 180 (± 2) °C, a composite catalyst of zinc acetate and n-butyl titanate dissolved in 0.9 mol of ethylene glycol is added, the temperature is raised to 230 (± 5) °C, and the reaction is carried out at the maintained temperature to ensure that the distillate amount of the fraction is greater than 95% of the theoretical amount.
[0053] After the temperature was further raised to 250 (± 2) °C, the introduction of N2 was stopped, and the vacuum was slowly evacuated to 5 Torr. Under this condition, the temperature and pressure were maintained to react until the resin viscosity reached 20000 (± 500) mPa.s, thereby obtaining a hydrophilic resin 4.
[0054] 2) N2 was introduced, the temperature was cooled to 160°C with stirring, 3% (mass fraction of the emulsion) of 1,3-dimethyl-2-imidazolidinone was added, the mixture was stirred fully, and the temperature was controlled to 130°C. The mixture was stirred for 1 hour at the temperature, and then the mixture was slowly discharged into an emulsifying kettle pre-filled with 70°C hot water and stirred and dispersed to complete the emulsification of the synthetic resin, thereby obtaining a washable water-absorbing quick-drying agent 4. The application effect is shown in Table 1.
[0055] Embodiment 5:
[0056] 1) 0.15 mol of PEG-3000 is added to a reaction kettle evacuated with N2 and equipped with a thermometer, a condensing device and a mechanical stirrer. After the reaction kettle is completely melted, 0.68 mol of ethylene terephthalate, 0.01 mol of glycerol and 0.51 mol of ethylene isophthalate are added and the mixture is heated to melt. When the temperature in the kettle rises to 180 (± 2) °C, a composite catalyst of zinc acetate and n-butyl titanate dissolved in 0.9 mol of ethylene glycol is added, the temperature is raised to 230 (± 5) °C, and the reaction is carried out at the maintained temperature to ensure that the distillate amount of the fraction is greater than 95% of the theoretical amount.
[0057] After the temperature was further raised to 250 (± 2) °C, the introduction of N2 was stopped, and the vacuum was slowly evacuated to 5 Torr. Under this condition, the temperature and pressure were maintained to react until the resin viscosity reached 20000 (± 500) mPa.s, thereby obtaining a hydrophilic resin 5.
[0058] 2) N2 was introduced, the temperature was cooled to 160°C with stirring, 3% (mass fraction of the emulsion) of 1,3-dimethyl-2-imidazolidinone was added, the mixture was stirred fully, and the temperature was controlled to 130°C. The mixture was stirred for 1 hour at the temperature, and then the mixture was slowly discharged into an emulsifying kettle pre-filled with 70°C hot water and stirred and dispersed to complete the emulsification of the synthetic resin, thereby obtaining a washable water-absorbing quick-drying agent 5. The application effect is shown in Table 1.
[0059] Embodiment 6:
[0060] 1) 0.15 mol of PEG-3000 is added to a reaction kettle evacuated with N2 and equipped with a thermometer, a condensing device and a mechanical stirrer. After the reaction kettle is completely melted, 0.68 mol of ethylene terephthalate, 0.01 mol of glycerol and 0.51 mol of ethylene isophthalate are added and the mixture is heated to melt. When the temperature in the kettle rises to 180 (± 2) °C, a composite catalyst of zinc acetate and n-butyl titanate dissolved in 0.9 mol of ethylene glycol is added, the temperature is raised to 230 (± 5) °C, and the reaction is carried out at the maintained temperature to ensure that the distillate amount of the fraction is greater than 95% of the theoretical amount.
[0061] After the temperature continues to rise to 250 (± 2) °C, the introduction of N2 is stopped, and the vacuum is slowly evacuated to 5 Torr. Under this condition, the temperature and pressure are maintained to react until the resin viscosity reaches 6000 (± 500) mPa.s, thereby obtaining a hydrophilic resin 6.
[0062] 2) N2 was introduced, the temperature was cooled to 160°C with stirring, 3% (mass fraction of the emulsion) of 1,3-dimethyl-2-imidazolidinone was added, the mixture was stirred fully, and the temperature was controlled to 130°C. The mixture was stirred for 1 hour at the temperature, and then the mixture was slowly discharged into an emulsifying kettle pre-filled with 70°C hot water and stirred and dispersed to complete the emulsification of the synthetic resin, thereby obtaining a washable water-absorbing quick-drying agent 6. The application effect is shown in Table 1.
[0063] Comparative Example 1:
[0064] 1) 0.15 mol of PEG-3000 is added to a reaction kettle evacuated with N2 and equipped with a thermometer, a condensing device and a mechanical stirrer. After the reaction kettle is completely melted, 0.68 mol of ethylene terephthalate, 0.01 mol of triethanolamine and 0.17 mol of ethylene isophthalate are added and the mixture is heated to melt. When the temperature in the kettle rises to 180 (± 2) °C, a composite catalyst of zinc acetate and n-butyl titanate dissolved in 0.9 mol of ethylene glycol is added, the temperature is raised to 230 (± 5) °C, and the reaction is carried out at the maintained temperature to ensure that the distillate amount of the fraction is greater than 95% of the theoretical amount.
[0065] After the temperature was further raised to 250 (± 2) °C, the introduction of N2 was stopped, and the vacuum was slowly evacuated to 5 Torr. Under this condition, the temperature and pressure were maintained to react until the resin viscosity reached 20000 (± 500) mPa.s, thereby obtaining hydrophilic resin 7.
[0066] 2) The hydrophilic resin 7 cannot be emulsified.
[0067] Comparative Example 2:
[0068] 1) 0.15 mol of PEG-3000 is added to a reaction kettle evacuated with N2 and equipped with a thermometer, a condensing device and a mechanical stirrer. After the reaction kettle is completely melted, 0.68 mol of ethylene terephthalate, 0.01 mol of citric acid and 0.17 mol of ethylene isophthalate are added and the temperature is raised to melt. When the temperature in the kettle rises to 180 (± 2) ° C, a composite catalyst of zinc acetate and n-butyl titanate dissolved in 0.9 mol of ethylene glycol is added, the temperature is raised to 230 (± 5) ° C, and the reaction is carried out at the maintained temperature to ensure that the distillate amount of the fraction is greater than 95% of the theoretical amount.
[0069] After the temperature was further raised to 250 (± 2) °C, the introduction of N2 was stopped, and the vacuum was slowly evacuated to 5 Torr. Under this condition, the temperature and pressure were maintained to react until the resin viscosity reached 20000 (± 500) mPa.s, thereby obtaining a hydrophilic resin 8.
[0070] 2) The hydrophilic resin 8 cannot be emulsified.
[0071] Comparative Example 3:
[0072] 1) In a reaction kettle evacuated with N2 and equipped with a thermometer, a condensing device and a mechanical stirrer, 0.08 mol of PEG-3000 is added, and after complete melting, 0.68 mol of ethylene terephthalate, 0.01 mol of glycerol and 0.17 mol of ethylene isophthalate are added, and the temperature is raised to melt; when the temperature in the kettle rises to 180 (± 2) ° C, a composite catalyst of zinc acetate and n-butyl titanate dissolved in 0.9 mol of ethylene glycol is added, and the temperature is raised to 230 (± 5) ° C, and the temperature is maintained for reaction to ensure that the distillate amount of the fraction is greater than 95% of the theoretical amount;
[0073] After the temperature was further raised to 250 (± 2) °C, the introduction of N2 was stopped, and the vacuum was slowly evacuated to 5 Torr. Under this condition, the temperature and pressure were maintained to react until the resin viscosity reached 20000 (± 500) mPa.s, thereby obtaining a hydrophilic resin 9.
[0074] 2) N2 was introduced, the temperature was cooled to 160°C with stirring, 3% (mass fraction of the emulsion) of 1,3-dimethyl-2-imidazolidinone was added, the mixture was stirred fully, and the temperature was controlled to 130°C. The mixture was stirred for 1 hour at the temperature, and then the mixture was slowly discharged into an emulsifying kettle pre-filled with 70°C hot water and stirred and dispersed to complete the emulsification of the synthetic resin, thereby obtaining a washable water-absorbing quick-drying agent 7, the application effect of which is shown in Table 1.
[0075] Comparative Example 4:
[0076] 1) In a reaction kettle evacuated with N2 and equipped with a thermometer, a condensing device and a mechanical stirrer, 5.13 mol of PEG-3000 is added, and after complete melting, 0.68 mol of ethylene terephthalate, 0.01 mol of glycerol and 0.17 mol of ethylene isophthalate are added, and the temperature is raised to melt; when the temperature in the kettle rises to 180 (± 2) ° C, a composite catalyst of zinc acetate and n-butyl titanate dissolved in 0.9 mol of ethylene glycol is added, and the temperature is raised to 230 (± 5) ° C, and the temperature is maintained for reaction to ensure that the distillate amount of the fraction is greater than 95% of the theoretical amount;
[0077] After the temperature was further raised to 250 (± 2) °C, the introduction of N2 was stopped, and the vacuum was slowly evacuated to 5 Torr. Under this condition, the temperature and pressure were maintained to react until the resin viscosity reached 20000 (± 500) mPa.s, thereby obtaining a hydrophilic resin 10.
[0078] 2) N2 was introduced, the temperature was cooled to 160°C with stirring, 3% (mass fraction of the emulsion) of 1,3-dimethyl-2-imidazolidinone was added, the mixture was stirred fully, and the temperature was controlled to 130°C. The mixture was stirred for 1 hour at the temperature, and then the mixture was slowly discharged into an emulsifying kettle pre-filled with 70°C hot water and stirred and dispersed to complete the emulsification of the synthetic resin, thereby obtaining a washable water-absorbing quick-drying agent 8. The application effect is shown in Table 1.
[0079] Comparative Example 5:
[0080] 1) 0.15 mol of PEG-400 is added to a reaction kettle evacuated with N2 and equipped with a thermometer, a condensing device and a mechanical stirrer. After the reaction kettle is completely melted, 0.68 mol of ethylene terephthalate, 0.01 mol of glycerol and 0.17 mol of ethylene isophthalate are added and the mixture is heated to melt. When the temperature in the kettle rises to 180 (± 2) °C, a composite catalyst of zinc acetate and n-butyl titanate dissolved in 0.9 mol of ethylene glycol is added, the temperature is raised to 230 (± 5) °C, and the reaction is carried out at the maintained temperature to ensure that the distillate amount of the fraction is greater than 95% of the theoretical amount.
[0081] After the temperature is continued to rise to 250 (± 2) °C, the introduction of N2 is stopped, and the vacuum is slowly evacuated to 5 Torr. Under this condition, the temperature and pressure are maintained to react until the resin viscosity reaches 20000 (± 500) mPa.s, thereby obtaining a hydrophilic resin 11.
[0082] 2) N2 was introduced, the temperature was cooled to 160°C with stirring, 3% (mass fraction of the emulsion) of 1,3-dimethyl-2-imidazolidinone was added, the mixture was stirred fully, and the temperature was controlled to 130°C. The mixture was stirred for 1 hour at the temperature, and then the mixture was slowly discharged into an emulsifying kettle pre-filled with 70°C hot water and stirred and dispersed to complete the emulsification of the synthetic resin, thereby obtaining a washable water-absorbing quick-drying agent 9, the application effect of which is shown in Table 1.
[0083] Comparative Example 6:
[0084] 1) 0.15 mol of PEG-600 is added to a reaction kettle evacuated with N2 and equipped with a thermometer, a condensing device and a mechanical stirrer. After the mixture is completely melted, 0.68 mol of ethylene terephthalate, 0.01 mol of glycerol and 0.17 mol of ethylene isophthalate are added and the mixture is heated to melt. When the temperature in the kettle rises to 180 (± 2) °C, a composite catalyst of zinc acetate and n-butyl titanate dissolved in 0.9 mol of ethylene glycol is added, the temperature is raised to 230 (± 5) °C, and the reaction is carried out at the maintained temperature to ensure that the distillate amount of the fraction is greater than 95% of the theoretical amount.
[0085] After the temperature continues to rise to 250 (± 2) °C, the introduction of N2 is stopped, and the vacuum is slowly evacuated to 5 Torr. Under this condition, the temperature and pressure are maintained to react until the resin viscosity reaches 20000 (± 500) mPa.s, thereby obtaining a hydrophilic resin 12.
[0086] 2) N2 was introduced, the temperature was cooled to 160°C with stirring, 3% (mass fraction of the emulsion) of 1,3-dimethyl-2-imidazolidinone was added, the mixture was stirred fully, and the temperature was controlled to 130°C. The mixture was stirred for 1 hour at the temperature, and then the mixture was slowly discharged into an emulsifying kettle pre-filled with 70°C hot water and stirred and dispersed to complete the emulsification of the synthetic resin, thereby obtaining a washable water-absorbing quick-drying agent 10. The application effect is shown in Table 1.
[0087] Comparative Example 7:
[0088] 1) 0.15 mol of PEG-8000 is added to a reaction kettle evacuated with N2 and equipped with a thermometer, a condensing device and a mechanical stirrer. After the reaction kettle is completely melted, 0.68 mol of ethylene terephthalate, 0.01 mol of glycerol and 0.17 mol of ethylene isophthalate are added and the mixture is heated to melt. When the temperature in the kettle rises to 180 (± 2) °C, a composite catalyst of zinc acetate and n-butyl titanate dissolved in 0.9 mol of ethylene glycol is added, the temperature is raised to 230 (± 5) °C, and the reaction is carried out at the maintained temperature to ensure that the distillate amount of the fraction is greater than 95% of the theoretical amount.
[0089] After the temperature continues to rise to 250 (± 2) °C, the introduction of N2 is stopped, and the vacuum is slowly evacuated to 5 Torr. Under this condition, the temperature and pressure are maintained to react until the resin viscosity reaches 20000 (± 500) mPa.s, thereby obtaining a hydrophilic resin 13.
[0090] 2) N2 was introduced, the temperature was cooled to 160°C with stirring, 3% (mass fraction of the emulsion) of 1,3-dimethyl-2-imidazolidinone was added, the mixture was stirred fully, and the temperature was controlled to 130°C. The mixture was stirred for 1 hour at the temperature, and then the mixture was slowly discharged into an emulsifying kettle pre-filled with 70°C hot water and stirred and dispersed to complete the emulsification of the synthetic resin, thereby obtaining a washable water-absorbing quick-drying agent 11. The application effect thereof is shown in Table 1.
[0091] Comparative Example 8:
[0092] 1) In a reaction kettle evacuated with N2 and equipped with a thermometer, a condensing device and a mechanical stirrer, 0.15 mol of PEG-3000 is added, and after complete melting, 0.68 mol of ethylene terephthalate and 0.01 mol of propylene glycol are added, and the temperature is raised to melt; when the temperature in the kettle rises to 180 (± 2) ° C, a composite catalyst of zinc acetate and n-butyl titanate dissolved in 0.9 mol of ethylene glycol is added, and the temperature is raised to 230 (± 5) ° C. The reaction is maintained at the temperature to ensure that the distillate amount of the fraction is greater than 95% of the theoretical amount;
[0093] After the temperature continues to rise to 250 (± 2) °C, the introduction of N2 is stopped, and the vacuum is slowly evacuated to 5 Torr. Under this condition, the temperature and pressure are maintained to react until the resin viscosity reaches 20000 (± 500) mPa.s, thereby obtaining a hydrophilic resin 14.
[0094] 2) The hydrophilic resin 14 cannot be emulsified.
[0095] Comparative Example 9:
[0096] 1) 0.15 mol of PEG-3000 is added to a reaction kettle evacuated with N2 and equipped with a thermometer, a condensing device and a mechanical stirrer. After the reaction kettle is completely melted, 0.68 mol of ethylene terephthalate, 0.01 mol of glycerol and 0.17 mol of ethylene isophthalate are added and the mixture is heated to melt. When the temperature in the kettle rises to 180 (± 2) °C, a composite catalyst of zinc acetate and n-butyl titanate dissolved in 0.9 mol of ethylene glycol is added, the temperature is raised to 230 (± 5) °C, and the reaction is carried out at the maintained temperature to ensure that the distillate amount of the fraction is greater than 95% of the theoretical amount.
[0097] After the temperature continues to rise to 250 (± 2) °C, the introduction of N2 is stopped, and the vacuum is slowly evacuated to 5 Torr. Under this condition, the temperature and pressure are maintained to react until the resin viscosity reaches 2000 (± 500) mPa.s, thereby obtaining a hydrophilic resin 15.
[0098] 2) N2 was introduced, the temperature was cooled to 160°C with stirring, 3% (by mass fraction of the emulsion) of 1,3-dimethyl-2-imidazolidinone was added, the mixture was stirred fully, and the temperature was controlled to 130°C. The mixture was stirred for 1 hour at the temperature, and then the mixture was slowly discharged into an emulsifying kettle pre-filled with 70°C hot water and stirred and dispersed to complete the emulsification of the synthetic resin, thereby obtaining a washable water-absorbing quick-drying agent 12. The application effect is shown in Table 1.
[0099] Comparative Example 10:
[0100] 1) 0.15 mol of PEG-3000 is added to a reaction kettle evacuated with N2 and equipped with a thermometer, a condensing device and a mechanical stirrer. After the reaction kettle is completely melted, 0.68 mol of ethylene terephthalate, 0.01 mol of glycerol and 0.17 mol of ethylene isophthalate are added and the mixture is heated to melt. When the temperature in the kettle rises to 180 (± 2) °C, a composite catalyst of zinc acetate and n-butyl titanate dissolved in 0.9 mol of ethylene glycol is added, the temperature is raised to 230 (± 5) °C, and the reaction is carried out at the maintained temperature to ensure that the distillate amount of the fraction is greater than 95% of the theoretical amount.
[0101] After the temperature continues to rise to 250 (± 2) °C, the introduction of N2 is stopped, and the vacuum is slowly evacuated to 5 Torr. Under this condition, the temperature and pressure are maintained to react until the resin viscosity reaches 35000 (± 500) mPa.s, thereby obtaining a hydrophilic resin 16.
[0102] 2) N2 was introduced, the temperature was cooled to 160°C with stirring, 3% (mass fraction of the emulsion) of 1,3-dimethyl-2-imidazolidinone was added, the mixture was stirred fully, and the temperature was controlled to 130°C. The mixture was stirred for 1 hour at the temperature, and then the mixture was slowly discharged into an emulsifying kettle pre-filled with 70°C hot water and stirred and dispersed to complete the emulsification of the synthetic resin, thereby obtaining a washable water-absorbing quick-drying agent 13. The application effect thereof is shown in Table 1.
[0103] Comparative Example 11:
[0104] 1) 0.15 mol of PEG-3000 is added to a reaction kettle evacuated with N2 and equipped with a thermometer, a condensing device and a mechanical stirrer. After the reaction kettle is completely melted, 0.68 mol of ethylene terephthalate, 0.01 mol of glycerol and 0.17 mol of ethylene isophthalate are added and the mixture is heated to melt. When the temperature in the kettle rises to 180 (± 2) °C, a composite catalyst of zinc acetate and n-butyl titanate dissolved in 0.9 mol of ethylene glycol is added, the temperature is raised to 230 (± 5) °C, and the reaction is carried out at the maintained temperature to ensure that the distillate amount of the fraction is greater than 95% of the theoretical amount.
[0105] After the temperature was further raised to 250 (± 2) °C, the introduction of N2 was stopped, and the vacuum was slowly evacuated to 5 Torr. Under this condition, the temperature and pressure were maintained to react until the resin viscosity reached 20000 (± 500) mPa.s, thereby obtaining a hydrophilic resin 1.
[0106] 2) N2 was introduced, the temperature was cooled to 160°C with stirring, 3% (by mass fraction of the emulsion) of ethylene glycol was added, the mixture was stirred fully, and the temperature was controlled to 130°C. The mixture was stirred for 1 hour at the temperature, and then the mixture was slowly discharged into an emulsifying kettle pre-filled with 70°C hot water and stirred and dispersed to complete the emulsification of the synthetic resin, thereby obtaining a washable water-absorbing quick-drying agent 14. The application effect thereof is shown in Table 1.
[0107] Comparative Example 12:
[0108] 1) 0.15 mol of PEG-3000 is added to a reaction kettle evacuated with N2 and equipped with a thermometer, a condensing device and a mechanical stirrer. After the reaction kettle is completely melted, 0.68 mol of ethylene terephthalate, 0.01 mol of glycerol and 0.17 mol of ethylene isophthalate are added and the mixture is heated to melt. When the temperature in the kettle rises to 180 (± 2) °C, a composite catalyst of zinc acetate and n-butyl titanate dissolved in 0.9 mol of ethylene glycol is added, the temperature is raised to 230 (± 5) °C, and the reaction is carried out at the maintained temperature to ensure that the distillate amount of the fraction is greater than 95% of the theoretical amount.
[0109] After the temperature was further raised to 250 (± 2) °C, the introduction of N2 was stopped, and the vacuum was slowly evacuated to 5 Torr. Under this condition, the temperature and pressure were maintained to react until the resin viscosity reached 20000 (± 500) mPa.s, thereby obtaining a hydrophilic resin 1.
[0110] 2) N2 was introduced, the temperature was cooled to 160°C with stirring, 3% (by mass fraction of the emulsion) of diethylene glycol was added, the mixture was stirred fully, and the temperature was controlled to 130°C. The mixture was stirred for 1 hour at the temperature, and then the mixture was slowly discharged into an emulsifying kettle pre-filled with 70°C hot water, and stirred and dispersed to complete the emulsification of the synthetic resin, thereby obtaining a washable water-absorbing quick-drying agent 15. The application effect is shown in Table 1.
[0111] Comparative Example 13:
[0112] 1) 0.15 mol of PEG-3000 is added to a reaction kettle evacuated with N2 and equipped with a thermometer, a condensing device and a mechanical stirrer. After the reaction kettle is completely melted, 0.68 mol of ethylene terephthalate, 0.01 mol of glycerol and 0.17 mol of ethylene isophthalate are added and the mixture is heated to melt. When the temperature in the kettle rises to 180 (± 2) °C, a composite catalyst of zinc acetate and n-butyl titanate dissolved in 0.9 mol of ethylene glycol is added, the temperature is raised to 230 (± 5) °C, and the reaction is carried out at the maintained temperature to ensure that the distillate amount of the fraction is greater than 95% of the theoretical amount.
[0113] After the temperature was further raised to 250 (± 2) °C, the introduction of N2 was stopped, and the vacuum was slowly evacuated to 5 Torr. Under this condition, the temperature and pressure were maintained to react until the resin viscosity reached 20000 (± 500) mPa.s, thereby obtaining a hydrophilic resin 1.
[0114] 2) N2 was introduced, the temperature was cooled to 160°C with stirring, 3% (by mass fraction of the emulsion) of isohexylene glycol was added, the mixture was stirred fully, and the temperature was controlled to 130°C. The mixture was stirred for 1 hour at the temperature, and then the mixture was slowly discharged into an emulsifying kettle pre-filled with 70°C hot water, and stirred and dispersed to complete the emulsification of the synthetic resin, thereby obtaining a washable water-absorbing quick-drying agent 16. The application effect is shown in Table 1.
[0115] Test example:
[0116] The wet rubbing color fastness evaluation method of the washable water-absorbing quick-drying finishing agents prepared in the above examples and comparative examples was evaluated with reference to the standard JIS-L-0849.
[0117] The finishing method of the evaluation fabric sample is as follows: for PET fabric, 3% Disperse Blue 79# or 2% Disperse Red 167# or 2% Disperse Orange 30# are used for the fabric weight, and dyeing is performed according to the conventional polyester fiber dyeing process to obtain dyed fabric; the finishing agent is used in an amount of 40 g / L, and a one-dip and one-roll finishing process is used for post-finishing; then, heat-set at 170°C for 60 seconds to obtain an evaluation fabric sample.
[0118] The quick-drying properties of the wash-resistant water-absorbing quick-drying finishing agents prepared in the above embodiments and comparative examples were evaluated according to the diffusive water residual rate test.
[0119] The test of drip diffusion time refers to the specific method in GBT 21655.1-2008 Evaluation of water absorption and quick-drying properties of textiles Part 1 Single item combined test method;
[0120] The specific operation method of the diffusive moisture residual rate (residual water rate) test method is as follows: take a 10cm×10cm size of the test fabric (avoid the edges, defects and wrinkles), and adjust the humidity for at least 4 hours under the conditions of T=20±2℃, RH=65±2%; accurately absorb 0.3mL of distilled water and drop it on the surface of the test fabric sample (skin-friendly side), test the mass of the fabric sample after each equal interval, and calculate the moisture residual rate according to the following formula:
[0121] Residual moisture rate (%) = (W0-W') / (W t -W′)×100
[0122] Where: W0 is the initial mass of the test fabric sample after water is added;
[0123] W t The mass of the test fabric sample at time t after water is added;
[0124] W' is the weight of the cloth.
[0125] The hydrophilic resins prepared in the above embodiments and comparative examples are evaluated as emulsifiable (which are divided into three grades: good, better and poor) if they can be normally dispersed in water after melting to form an emulsion with a smaller particle size; if they cannot be completely dispersed or do not disperse in water, they are evaluated as unemulsifiable.
[0126] The PET fabric is 100% polyester knitted fabric (weight: 140g / m 2 ).
[0127] The disperse dyes used in the evaluation, 79# Disperse Blue, 167# Disperse Red, and 30# Disperse Orange, are all readily available commercial products.
[0128] The washing process of the finished fabric was carried out according to JIS L 0217103 method.
[0129] The rubbing color fastness of the finished dyed fabrics was tested according to JIS L 0849.
[0130] The model of the commercially available product is NICEPOLE PR-100 (produced by Nichia Chemical (China) Co., Ltd.) Table 1 Emulsification properties of hydrophilic resins and padding and finishing properties of corresponding hydrophilic quick-drying agents
[0131]
[0132] The comparison between Examples 1 and 2 and Comparative Examples 1 and 2 indicates that different multifunctional monomers play a key role in the design process of the functional resin. The dosage, type and order of addition of the multifunctional monomer or the mixture of multifunctional monomers selected in the invention have a significant impact on the emulsification and final performance of the hydrophilic quick-drying agent in the invention, and the examples and comparative examples only point out the simplest application method.
[0133] Compared with Example 2, Examples 3-5 and Comparative Examples 3-8 provide possible changes in various monomers, raw materials and corresponding specifications in the resin of the present invention, and point out the influence of various factors on the application effect of the final resin. By comparing Examples 2, 5 and Comparative Example 8, it can be seen that by controlling the molar feed ratio of ethylene terephthalate to ethylene isophthalate and or sodium 1,3-dimethyl phthalate-5-sulfonate, the molecular regularity of the block polyester polyether resin can be adjusted, thereby improving the emulsification;
[0134] The comparison between Example 2 and Comparative Examples 11, 12 and 13 shows the effect of solvent screening. A suitable solvent can not only improve the emulsification performance of the inventive resin, but also does not lose its original excellent performance.
[0135] It should also be noted that the various specific technical features described in the above specific embodiments can be combined in any suitable manner without contradiction. In order to avoid unnecessary repetition, the present invention will not further describe various possible combinations.
Claims
1. A high-fastness, high-washing-resistant, water-absorbing and quick-drying resin, characterized in that: The resin is a low-branched block polyester polyether hydrophilic resin containing a multifunctional small molecular monomer structure, and the structure is as follows: Wherein, m, n, a, b, c are all natural numbers, 1≤m≤150, 1≤n≤4, 1≤a+b+c≤30; X is a monomer structure with a functionality ≥3; The functionality of the resin is ≥3.
2. A high-fastness, high-washing-resistant, water-absorbing and quick-drying resin according to claim 1, characterized in that: The molar number of multifunctional small molecule monomers in the low-branching block polyester polyether hydrophilic resin accounts for 0.1%-40% of the molar number of total monomers.
3. A high-fastness, high-washing-resistant, water-absorbing and quick-drying resin according to claim 2, characterized in that: The molar ratio of the total monomers is 0.5-20%.
4. The high-fastness, high-washing-resistant, water-absorbing and quick-drying resin according to claim 1, characterized in that: The multifunctional monomer is a small molecule monomer, and the functional groups in the monomer include one or more of hydroxyl, carboxyl, and amino.
5. A high-fastness, high-washing-resistant, water-absorbing and quick-drying resin according to claim 4, characterized in that: The multifunctional small molecule monomer is a polyol or a polycarboxylic acid or a triamine or a mixed monomer thereof.
6. A high-fastness, high-washing-resistant, water-absorbing and quick-drying resin according to claim 5, characterized in that: The multifunctional small molecule monomer is a mixture of one or more of glycerol, triethanolamine, pentaerythritol and trimethylolpropane, dimethylolpropionic acid, dimethylolbutyric acid, pyromellitic anhydride and citric acid.
7. The high-fastness, high-washing-resistant, water-absorbing and quick-drying resin according to claim 1, characterized in that: The low-branching block polyester polyether hydrophilic resin has a melt viscosity of 3000-60000 mPa·s.
8. The use of a high-fastness, high-washing-resistant, water-absorbing and quick-drying resin according to claim 1, characterized in that: By post-finishing the fabric, a fiber product containing a low-branching block polyester polyether hydrophilic resin component in an amount of 0.01-10% owf is obtained.
9. The use of a high-fastness, high-washing-resistant, water-absorbing and quick-drying resin according to claim 8, characterized in that: The finishing methods include but are not limited to dyeing in one bath, dyeing in bath and post-dyeing padding and finalizing treatment; The fabric is mainly PET fabric or a fabric prepared by any spinning and weaving process using PET fiber and other fibers and is subjected to water absorption and quick-drying finishing.
