Full-dull porous PTT fiber and preparation method thereof

By using amino-containing mesoporous titanium dioxide powder in PTT fiber production, the problems of acrolein production and release during spinning are solved, and the effect of low acrolein content and safety improvement is achieved.

CN119265741APending Publication Date: 2025-01-07JIANGSU XUANDA POLYMER MATERIAL CO LTD
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Patent Information

Application Number
CN202411462719.7
Authority / Receiving Office
CN · China
Patent Type
Applications(China)
Current Assignee / Owner
Filing Date
2024-10-19
Publication Date
2025-01-07

AI Technical Summary

Technical Problem

During the PTT spinning process, the production and release of acrolein leads to deterioration of the production environment, and the existing cleaning methods are inefficient or have safety risks.

Method used

The amino-containing mesoporous titanium dioxide powder is introduced as a matting agent and acrolein scavenger, which reduces the formation and release of acrolein through its porous structure adsorption and chemical bonding reaction.

Benefits of technology

It effectively reduces the acrolein content in PTT fibers, improves the production environment, improves the spinning and dyeing conditions, and enhances the safety of the fibers.

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Abstract

The invention discloses a full-dull porous PTT fiber, the raw materials of the full-dull porous PTT fiber comprise PTT polyester and a delustering agent, the delustering agent is mesoporous titanium dioxide powder, the aperture of the mesoporous titanium dioxide powder is 2-4 nm, the specific surface area is 100-300 m < 2 > / g, the particle size is 200-300 nm, and the surface of the mesoporous titanium dioxide powder contains 1-3 wt% of amino functional groups. The invention also discloses a preparation method of the full-dull porous PTT fiber. The preparation method comprises the following steps: preparing the mesoporous titanium dioxide powder; and mixing terephthalic acid, 1, 3-propylene glycol and the mesoporous titanium dioxide powder to react to prepare PTT polyester, then pelletizing to obtain PTT polyester chips, and then metering, extruding, cooling, oiling, stretching and winding the PTT polyester chips to prepare the full-dull porous PTT fiber. According to the preparation method disclosed by the invention, the release of acrolein steam can be reduced in the preparation process, the production environment is improved, and the obtained PTT fibers are low in acrolein content and beneficial to the safety of subsequent spinning, dyeing and service.
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Claims

1. A fully matte porous PTT fiber, characterized in that: The raw materials of the fully matte porous PTT fiber include PTT polyester and a matting agent, wherein the matting agent is mesoporous titanium dioxide powder, and the pore size of the mesoporous titanium dioxide powder is 2-4 nm, and the specific surface area is 100-300 m 2 / g, a particle size of 200-300nm, and the surface of the mesoporous titanium dioxide powder contains 1-3wt% of amino functional groups.

2. The method for preparing the fully matte porous PTT fiber according to claim 1, characterized in that: The following steps are involved: The mesoporous titanium dioxide powder is prepared; Terephthalic acid, 1,3-propylene glycol and the mesoporous titanium dioxide powder are mixed and reacted to obtain PTT polyester, which is then pelletized to obtain PTT polyester chips, which are then metered, melted, extruded, cooled, oiled, stretched and wound to obtain the fully matte porous PTT fiber.

3. The method for preparing the fully matte porous PTT fiber according to claim 2, characterized in that: The intrinsic viscosity of the PTT polyester chips is 1.10-1.20 dL / g, and the content of the mesoporous titanium dioxide powder is 2.0-2.2 wt %.

4. The method for preparing the fully matte porous PTT fiber according to claim 2, characterized in that: The specific steps of preparing the PTT polyester are as follows: After terephthalic acid, 1,3-propylene glycol and the mesoporous titanium dioxide powder are prepared into a slurry, an esterification reaction is carried out at a temperature of 230-250° C. and a reaction time of 70-90 minutes. When the amount of water distilled in the esterification reaction reaches more than 95% of the theoretical value, the esterification reaction ends, and an esterified product is obtained; A catalyst and a stabilizer are added to the esterified product, and a polycondensation reaction in a low vacuum stage is started under negative pressure. The pressure in this stage is steadily pumped from normal pressure to an absolute pressure below 500 Pa, the temperature is controlled at 260-270° C., and the reaction time is 30-50 minutes. Then, the vacuum is continued to be pumped to carry out a polycondensation reaction in a high vacuum stage. The pressure in this stage reduces the reaction pressure to an absolute pressure of less than 70 Pa, the reaction temperature is controlled at 270-275° C., and the reaction time is 50-90 minutes to obtain the PTT polyester.

5. The method for preparing the fully matte porous PTT fiber according to claim 4, characterized in that: The molar ratio of terephthalic acid to 1,3-propylene glycol is 1:(1.3-1.5).

6. The method for preparing the fully matte porous PTT fiber according to claim 4, characterized in that: The catalyst is tetrabutyl titanate, tetraisopropyl titanate, tetraethyl titanate, stannous acetate or dibutyltin diacetate, and the added amount of the catalyst is 0.02%-0.03% of the total weight of terephthalic acid. The stabilizer is triphenyl phosphate, trimethyl phosphate or trimethyl phosphite, and the added amount of the stabilizer is 0.01%-0.03% of the total weight of the terephthalic acid.

7. The method for preparing the fully matte porous PTT fiber according to claim 4, characterized in that: The specific steps for preparing the mesoporous titanium dioxide powder are as follows: Using alkylamine as a template agent and isopropyl titanate or n-butyl titanate as a titanium source, the template agent and the titanium source are mixed and dissolved in ethanol, deionized water is added to generate a precipitate, and a portion of the template agent is removed by aging, filtering, and extraction, and the mesoporous titanium dioxide powder is obtained by washing and drying; The alkylamine is one of dodecaamine, tetradecaamine, hexadecaamine and octadecylamine, the molar ratio of the alkylamine to the titanium source is 1:(2-3), the volume ratio of ethanol to deionized water is 1:(4-5), and the concentration of the alkylamine is 2-2.2 wt%.

8. The method for preparing the fully matte porous PTT fiber according to claim 7, characterized in that: The aging conditions are: first at room temperature, keep warm for 20-24 hours, then heat to 90-100°C, keep warm for 40-48 hours; The extraction conditions are as follows: treatment in a nitric acid ethanol solution at pH = 2 at room temperature for 12-15 hours; The washing conditions are: ethanol filtration and washing 3-5 times; The drying conditions are as follows: drying temperature is 50-60° C., and drying time is 24-30 hours.

9. The method for preparing the fully matte porous PTT fiber according to claim 4, characterized in that: Extrusion temperature 270-280℃, cooling temperature 20-25℃, cooling wind speed 1.80-2.30m / s, first roller speed 1800-2000m / min, first roller temperature 70-80℃, second roller speed 3000-3300m / min, second roller temperature 140-150℃, winding speed 2930-3210m / min.

10. The method for preparing the fully matte porous PTT fiber according to claim 4, characterized in that: The breaking strength of the fully matte porous PTT fiber is ≥3.5 cN / dtex, the breaking elongation is 40.0±5.0%, the single fiber fineness is 0.6-0.8 dtex, the glossiness is <30%, and the acrolein content in the fully matte porous PTT fiber is <1.5 ppm.

Citation Information

Patent Citations

  • A crystalline low-melting-point polyester fiber and its preparation method

    CN106811829B

  • Acrolein scavenging in ptf and other 1,3-propanediol derived polymers

    CN109996830A