Preparation method of cationic dyeable PET (Polyethylene Terephthalate) fiber and cationic dyeable PET fiber
Through the preparation method of cationic dyeable PET, the problems of uneven dyeing and low dyeing in PET fiber dyeing are solved, and the effects of uniform dyeing and high dyeing are achieved. They are suitable for large-scale production and perform well in water resistance and light resistance color fastness detection.
Patent Information
- Application Number
- CN202411556789.9
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2024-11-01
- Publication Date
- 2025-03-07
AI Technical Summary
There are problems of uneven dyeing and low dyeing during the dyeing and finishing of existing PET fibers, which leads to inconsistent dyeing and restricts its large-scale production and use.
The preparation method of cationic dyeable PET is adopted, including beating a mixture containing titanium dioxide, terephthalic acid and ethylene glycol, passing esterification reaction, pre-polycondensation reaction and melt blending, adding benzene sulfonate compound, and then mixing with a filler to obtain cationic dyeable PET fibers. The method includes spinning, cooling and curing and winding forming steps, controlling the spinning temperature between 180 and 280°C, and adjusting the cooling and curing temperature, wind speed and relative humidity within a specific range.
It achieves uniform dyeing, high dyeing degree, excellent fiber performance, and is suitable for large-scale production. Cationic dyeable PET fibers do not fade in the detection of water-resistant and light-resistant color fastness, and have high dyeing.
Smart Images
Figure BDA0005117712530000051
Abstract
Description
Technical Field
[0001] The present application relates to a preparation method of a cationically dyeable PET fiber and the cationically dyeable PET fiber, belonging to the technical field of fiber dyeing production. Background Art
[0002] The importance of chemical fiber in modern life is self-evident. It not only meets people's demand for the diversification and functionality of textiles, but also promotes the progress of textile technology and the development of the industry. The chemical fiber industry continues to promote the research and development of new materials and technologies, such as environmentally friendly fibers, functional fibers, and smart fibers, providing new impetus for the development of the textile industry.
[0003] At present, in the dyeing and finishing process of PET fiber, there are problems such as uneven dyeing and low dyeing degree, which cannot achieve uniform dyeing, limiting its large-scale production and use. Therefore, the present application provides a dyeing and finishing process to solve the problems of uneven dyeing and uneven dyeing in the existing dyeing and finishing. Summary of the invention
[0004] The present application provides a method for preparing cationic dyeable PET fibers, which effectively achieves uniform dyeing and high dyeing degree, and the prepared fibers have good performance and are conducive to large-scale production.
[0005] According to one aspect of the present application, a method for preparing a cationic dyeable PET fiber is provided, the preparation method comprising the following steps:
[0006] S1: preparing a cationic dyeable PET melt by using cationic dyeable PET;
[0007] S2: spinning, cooling, solidifying, and winding the cationic dyeable PET melt to obtain the cationic dyeable PET fiber;
[0008] In the step S2, the spinning temperature is 180-280°C.
[0009] Optionally, in step S2, the spinning temperature is independently selected from any value of 180°C, 200°C, 220°C, 240°C, 250°C, 260°C, 280°C or a range between any two of the above values.
[0010] Optionally, the temperature of cooling and curing is 5 to 45° C., the wind speed of cooling and curing is 0.2 to 1.2 m / s, and the relative humidity of cooling and curing is 50 to 85%.
[0011] Optionally, the cooling and curing temperature is independently selected from any value of 5°C, 10°C, 15°C, 20°C, 25°C, 30°C, 35°C, 40°C, 45°C or a range between any two of the above values.
[0012] Optionally, the wind speed for cooling and solidification is independently selected from any value among 0.2m / s, 0.4m / s, 0.6m / s, 0.8m / s, 1m / s, 1.2m / s or a range between any two of the above values.
[0013] Optionally, in step S2, the guide wire speed of the winding forming is 2000-2800 m / min, and the winding speed of the winding forming is 2000-2800 m / min.
[0014] Optionally, in step S2, the guide wire speed for winding is independently selected from any value among 2000m / min, 2100m / min, 2200m / min, 2300m / min, 2400m / min, 2500m / min, 2600m / min, 2700m / min, 2800m / min or a range value between any two of the above.
[0015] Optionally, in step S2, the winding speed of the winding molding is independently selected from any value among 2000m / min, 2100m / min, 2200m / min, 2300m / min, 2400m / min, 2500m / min, 2600m / min, 2700m / min, 2800m / min or a range value between any two of the above.
[0016] Optionally, in step S1, the method for preparing the cationic dyeable PET comprises the following steps:
[0017] (1) beating a mixture containing titanium dioxide, terephthalic acid, and ethylene glycol to obtain a slurry;
[0018] (2) subjecting the slurry to esterification reaction and pre-polycondensation reaction respectively to obtain a pre-polycondensation product;
[0019] (3) adding a benzenesulfonate compound to the pre-polycondensation product, and melt blending the mixture to obtain a cationic dyeable PET precursor;
[0020] (4) mixing the cationic dyeable PET precursor and the filler, and reacting them to obtain the cationic dyeable PET.
[0021] Optionally, the pre-polycondensation reaction includes pre-polycondensation reaction I and pre-polycondensation reaction II;
[0022] The temperature of the pre-polycondensation reaction I is 100-190° C., the vacuum degree of the pre-polycondensation reaction I is 50-450 Pa, and the time of the pre-polycondensation reaction I is 0.5-5 h;
[0023] The temperature of the pre-polycondensation reaction II is 150-260° C., the vacuum degree of the pre-polycondensation reaction II is 100-600 Pa, and the time of the pre-polycondensation reaction II is 1h-6h.
[0024] Optionally, the benzenesulfonate compound is selected from sodium dimethyl 5-sulfonate isophthalate and / or sodium dimethyl 5-sulfonate terephthalate.
[0025] Optionally, the melt blending temperature is 235 to 250° C., and the melt blending time is 10 to 40 minutes.
[0026] Optionally, the mass fraction of the titanium dioxide in the slurry is 0.8-2.5%.
[0027] Optionally, the molar ratio of the terephthalic acid to the ethylene glycol is 1:(1-1.3).
[0028] Optionally, the molar ratio of the benzenesulfonate compound to the terephthalic acid is (0.01-0.5):1.
[0029] Optionally, the filler is selected from at least one of SiO2, TiO2 and montmorillonite.
[0030] Optionally, the mass fraction of the filler in the cationic dyeable PET precursor is 2% to 10%.
[0031] Optionally, the pressure of the esterification reaction is 0.3-0.6 MPa, the temperature of the esterification reaction is 220-240° C., and the time of the esterification reaction is 0.5-4 h.
[0032] Optionally, the reaction temperature is 100-300° C., and the reaction time is 1-5 h.
[0033] According to another aspect of the present application, a cationic dyeable PET fiber prepared by the above-mentioned preparation method is provided.
[0034] The beneficial effects of this application include:
[0035] The cationic dyeable PET fiber provided in this application can meet the dyeing and finishing of various colors and improve its dyeing degree to meet the needs of more clothing and home textile fields. When the spinning temperature is between 180 and 280°C, the spinning effect is good, and the cationic dyeable PET fiber does not fade in the water fastness and light fastness tests, has a high dyeing degree, and the prepared fiber has good performance, which is conducive to large-scale production. DETAILED DESCRIPTION
[0036] The present application is described in detail below with reference to embodiments, but the present application is not limited to these embodiments.
[0037] Unless otherwise specified, the raw materials in the examples of this application were purchased through commercial channels.
[0038] Example 1
[0039] Titanium dioxide, terephthalic acid and ethylene glycol are placed in a pulping kettle, stirred and mixed at 120°C, the stirring speed is increased from 200 r / min to 1000 r / min within 20 minutes, and then maintained at 1000 r / min for 60 minutes to complete the pulping and prepare a slurry; wherein the mass fraction of titanium dioxide in the slurry is 0.8%, and the molar ratio of terephthalic acid to ethylene glycol is 1:1.
[0040] The slurry was esterified using nitrogen as the protective gas, the esterification pressure was controlled at 0.30 MPa, the esterification temperature was 220°C, and the esterification time was 0.5 h. When the water output reached 80% of the theoretical water output, the esterification was continued at 240°C and normal pressure for 1 h. After the esterification was completed, the esterification product was prepared.
[0041] The esterification product was subjected to a pre-condensation reaction, the pre-condensation temperature was controlled to be 100°C, the pre-condensation vacuum was 50Pa, and the pre-condensation time was 0.5h. The temperature was then raised to 200°C again, the pre-condensation vacuum was maintained at 100Pa, and the pre-condensation reaction was continued for 1h to obtain a pre-condensation product.
[0042] Add sodium bis(hydroxypropyl)-5-sulfonate isophthalate to the precondensation product, and then perform melt blending with nitrogen as protective gas, control the melt blending temperature to be 235° C., and the melt blending time to be 10 min to prepare a cationic dyeable PET precursor (the intrinsic viscosity of the initial product of the cationic dyeable PET is about 0.3 dL / g); wherein the molar ratio of sodium bis(hydroxypropyl)-5-sulfonate isophthalate to terephthalic acid is 0.01:1.
[0043] The cationic dyeable PET precursor is reacted with SiO2 microcrystals, wherein the amount of SiO2 microcrystals is 2% of the mass of the cationic dyeable PET precursor, the reaction temperature is 100° C., and the reaction time is 1 hour, to obtain the cationic dyeable PET.
[0044] Example 2
[0045] The cationic dyeable PET prepared in Example 1 was melt-extruded through a screw, and the melt entered a spinning box. The temperature of the PET spinning box was controlled to be 180° C., the cooling and curing temperature was controlled to be 5° C., the wind speed was 0.2 m / s, and the relative humidity was 50%. After cooling, the filaments were wound. During the winding, the wire guide speed was 2000 m / min and the winding speed was 2000 m / min, and finally the cationic dyeable PET fiber was prepared.
[0046] Example 3
[0047] The cationic dyeable PET prepared in Example 1 was melt-extruded through a screw, and the melt entered a spinning box. The temperature of the PET spinning box was controlled to be 280° C., the cooling and curing temperature was controlled to be 45° C., the wind speed was 1.2 m / s, and the relative humidity was 85%. After cooling, the filaments were wound. During the winding, the wire guide speed was 2800 m / min and the winding speed was 2800 m / min, and finally the cationic dyeable PET fiber was prepared.
[0048] Example 4
[0049] The cationic dyeable PET prepared in Example 1 was melt-extruded through a screw, and the melt entered a spinning box. The temperature of the PET spinning box was controlled to be 240° C., the cooling and curing temperature was controlled to be 25° C., the wind speed was 0.6 m / s, and the relative humidity was 65%. After cooling, the filaments were wound. During the winding, the wire guide speed was 2400 m / min and the winding speed was 2400 m / min, and finally the cationic dyeable PET fiber was prepared.
[0050] Comparative Example 1
[0051] The cationic dyeable PET prepared in Example 1 was melt-extruded through a screw, and the melt entered a spinning box. The temperature of the PET spinning box was controlled to be 170° C., the cooling and curing temperature was controlled to be 5° C., the wind speed was 0.2 m / s, and the relative humidity was 50%. After cooling, the filaments were wound. During the winding, the wire guide speed was 2000 m / min and the winding speed was 2000 m / min, and finally the cationic dyeable PET fiber was prepared.
[0052] Comparative Example 2
[0053] The cationic dyeable PET prepared in Example 1 was melt-extruded through a screw, and the melt entered a spinning box. The temperature of the PET spinning box was controlled to be 290° C., the cooling and curing temperature was controlled to be 5° C., the wind speed was 0.2 m / s, and the relative humidity was 50%. After cooling, the filaments were wound. During the winding, the wire guide speed was 2000 m / min and the winding speed was 2000 m / min, and finally the cationic dyeable PET fiber was prepared.
[0054] Test Example 1
[0055] The cationic dyeable PET fibers prepared in the examples and comparative examples were tested for color fastness to water and color fastness to light. The test results are shown in Table 1.
[0056]
[0057]
[0058] It can be seen from Table 1 that when the spinning temperature is between 180 and 280°C, the spinning effect is better, the cationic dyeable PET fiber does not fade in the water fastness and light fastness tests, the dyeing degree is high, the prepared fiber has good performance, and is conducive to large-scale production.
[0059] The above are only a few embodiments of the present application and do not constitute any form of limitation to the present application. Although the present application is disclosed as above with preferred embodiments, it is not intended to limit the present application. Any technician familiar with the profession, without departing from the scope of the technical solution of the present application, using the technical content disclosed above to make slight changes or modifications are equivalent to equivalent implementation cases and fall within the scope of the technical solution.
Claims
1. A method for preparing a cationic dyeable PET fiber, characterized in that: The preparation method comprises the following steps: S1: preparing a cationic dyeable PET melt by using cationic dyeable PET; S2: spinning, cooling, solidifying, and winding the cationic dyeable PET melt to obtain the cationic dyeable PET fiber; In the step S2, the spinning temperature is 180-280°C.
2. The preparation method according to claim 1, characterized in that: The temperature of cooling and curing is 5-45° C., the wind speed of cooling and curing is 0.2-1.2 m / s, and the relative humidity of cooling and curing is 50-85%.
3. The preparation method according to claim 1, characterized in that: In the step S2, the guide wire speed of the winding forming is 2000-2800 m / min, and the winding speed of the winding forming is 2000-2800 m / min.
4. The preparation method according to claim 1, characterized in that: In step S1, the method for preparing the cationic dyeable PET comprises the following steps: (1) beating a mixture containing titanium dioxide, terephthalic acid, and ethylene glycol to obtain a slurry; (2) subjecting the slurry to esterification reaction and pre-polycondensation reaction respectively to obtain a pre-polycondensation product; (3) adding a benzenesulfonate compound to the pre-polycondensation product, and melt blending the mixture to obtain a cationic dyeable PET precursor; (4) mixing the cationic dyeable PET precursor and the filler, and reacting them to obtain the cationic dyeable PET.
5. The preparation method according to claim 4, characterized in that: The pre-polycondensation reaction includes pre-polycondensation reaction I and pre-polycondensation reaction II; The temperature of the pre-polycondensation reaction I is 100-190° C., the vacuum degree of the pre-polycondensation reaction I is 50-450 Pa, and the time of the pre-polycondensation reaction I is 0.5-5 h; The temperature of the pre-polycondensation reaction II is 150-260° C., the vacuum degree of the pre-polycondensation reaction II is 100-600 Pa, and the time of the pre-polycondensation reaction II is 1h-6h.
6. The preparation method according to claim 4, characterized in that: The benzenesulfonate compound is selected from sodium dimethyl 5-sulfonate isophthalate and / or sodium dimethyl 5-sulfonate terephthalate; Preferably, the melt blending temperature is 235-250° C., and the melt blending time is 10-40 min.
7. The preparation method according to claim 4, characterized in that: The mass fraction of titanium dioxide in the slurry is 0.8-2.5%; Preferably, the molar ratio of the terephthalic acid to the ethylene glycol is 1:(1-1.3); Preferably, the molar ratio of the benzenesulfonate compound to the terephthalic acid is (0.01-0.5):
1.
8. The preparation method according to claim 4, characterized in that: The filler is selected from at least one of SiO2, TiO2 and montmorillonite; Preferably, the mass fraction of the filler in the cationic dyeable PET precursor is 2% to 10%.
9. The preparation method according to claim 4, characterized in that: The pressure of the esterification reaction is 0.3-0.6 MPa, the temperature of the esterification reaction is 220-240° C., and the time of the esterification reaction is 0.5-4 h; Preferably, the reaction temperature is 100-300° C., and the reaction time is 1-5 h.
10. Cationic dyeable PET fiber prepared by the preparation method according to any one of claims 1 to 9.