Bio-based synthetic fiber and wool blended fabric and preparation method thereof

The preparation method of bio-based synthetic fibers by combining compound microbial fermentation and ultrasonic-assisted crystallization, combined with compression polymerization under CO2 atmosphere and electrostatic melt spinning, solves the problems of low pretreatment efficiency and high polymerization energy consumption of bio-based synthetic fibers, and produces blended fabrics with excellent durability and elastic recovery, suitable for outdoor sportswear and casual woven fabrics.

CN121451353APending Publication Date: 2026-02-03SHAOXING HUASI NEW MATERIAL TECHNOLOGY CO LTD
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Patent Information

Application Number
CN202511682640.X
Authority / Receiving Office
CN · China
Patent Type
Applications(China)
Current Assignee / Owner
Filing Date
2025-11-17
Publication Date
2026-02-03

AI Technical Summary

Technical Problem

Existing bio-based synthetic fibers suffer from low pretreatment efficiency, long fermentation cycles, easy agglomeration of intermediate crystals, and high energy consumption in polymerization reactions, making it difficult to meet the mechanical requirements of blended fabrics and limiting their industrial application.

Method used

A composite microbial agent and a composite cell wall degrading enzyme were used to simultaneously ferment corn stalks. Combined with ultrasonic-assisted crystallization and compression polymerization under CO2 atmosphere, bio-based synthetic fibers were prepared. The fibers were then melt-spun by electrostatic field and liquid nitrogen quenching, and subsequently blended with wool to make fabric.

Benefits of technology

It improves the durability and elasticity recovery of blended fabrics, meets the standard requirements for appearance quality, has high resistance to pilling and fuzzing, and has excellent crease recovery angle and pleat durability, thus meeting the durability and appearance requirements of outdoor sportswear and casual woven fabrics.

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Abstract

The invention discloses a bio-based synthetic fiber and wool blended fabric and a preparation method thereof, and belongs to the technical field of textiles. The preparation method comprises the following steps: S1, mixing wool fibers with bio-based synthetic fibers, and sequentially performing opening, carding, drawing, roving and spinning procedures to prepare blended yarns; s2, weaving the blended yarns prepared in the step S1 into gray cloth through a tatting process; s3, the gray cloth obtained in the S2 is subjected to washing, fulling and shaping after-finishing procedures, and the blended fabric is obtained. The invention discloses a bio-based synthetic fiber and wool blended fabric and a preparation method thereof, the durability of the blended fabric is remarkably improved, the blended fabric has excellent elasticity recovery capability, and the appearance quality of a product meets the standard requirement.
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Description

TECHNICAL FIELD

[0001] The present application belongs to the technical field of textiles, and particularly relates to a blended fabric of bio-based synthetic fiber and wool and a preparation method thereof. BACKGROUND

[0002] With the improvement of environmental awareness, bio-based synthetic fibers made from agricultural waste have become a research hotspot in the textile field. The blended fabric of bio-based synthetic fibers and wool has a pressing demand in outdoor sports clothing, casual woven products and other scenarios due to its biodegradability and moisture absorption properties of wool. At present, the preparation of bio-based synthetic fibers is mostly made from agricultural waste such as corn stalks and sugarcane residues. However, the existing technology has significant defects. First, single enzymatic hydrolysis or single microbial fermentation process is often used in the pretreatment stage of biomass, such as using only cellulase for enzymatic hydrolysis (publication number CN114574238A) or relying only on yeast fermentation, which leads to low degradation efficiency of cellulose, hemicellulose and pectin in straw, and a long fermentation period of 48-72h. In addition, the product purity is insufficient, and the subsequent polymerization reaction is prone to produce by-products. Second, pure aqueous solution system is often used in the crystallization process of intermediates, and the crystals are prone to agglomeration, which requires multiple water washing and leads to large wastewater discharge. Third, high-temperature and high-pressure reactions under nitrogen protection are often used in the polymerization stage, which has high energy consumption and is prone to oxidative degradation of polymers, making it difficult to meet the mechanical requirements of blended fabrics and limiting its industrial application. SUMMARY

[0003] The present application aims to provide a blended fabric of bio-based synthetic fiber and wool and a preparation method thereof. The blended fabric has significantly improved durability and excellent elastic recovery ability, and the product appearance quality meets the standard requirements.

[0004] To solve the above technical problems, the technical solution adopted by the present application is as follows: A preparation method of a blended fabric of bio-based synthetic fiber and wool, comprising the following steps: S1, mixing wool fibers and bio-based synthetic fibers, and sequentially going through the processes of opening, carding, drawing, roving and spinning to produce blended yarns; S2, weaving the blended yarns produced in S1 into greige fabric through the weaving process; S3, obtaining the blended fabric after the greige fabric obtained in S2 goes through the processes of scouring, milling, setting and finishing.

[0005] Preferably, in S1, the mass ratio of wool fibers to bio-based synthetic fibers is (3-7):(2-8).

[0006] Preferably, the preparation process of bio-based synthetic fibers comprises the following steps: T1, corn stalks are dried, crushed, acid pretreated, and then inoculated with a compound microbial agent and a compound cell wall degrading enzyme for fermentation, and the fermentation liquor is centrifuged, membrane separated and ion exchanged to obtain a reaction product A; T2, the reaction product A obtained in step T1 is reacted with hexanediamine in an ethanol-water mixed solvent, and after the reaction is completed, ultrasonic assisted programmed cooling crystallization is used, and after filtration and drying, a reaction product B is obtained; T3, the reaction product B obtained in step T2 is prepared into an aqueous solution, and a pressurized polycondensation reaction is carried out under a CO2 atmosphere, including three stages of pre-polycondensation, pressure relief polycondensation and vacuum polycondensation, to obtain a reaction product C; T4, the reaction product C obtained in step T3 is dried and then melt spun, and an electrostatic field and liquid nitrogen micro-mist quenching are applied synchronously during the spinning process, and after oiling, winding and heat stretching, a bio-based synthetic fiber is obtained, thereby obtaining a bio-based synthetic fiber.

[0007] Preferably, in T1, the compound microbial agent is composed of yeast and bacillus, and the ratio of viable bacteria is (1-2):1; the compound cell wall degrading enzyme is composed of cellulase, pectinase and xylanase in a mass ratio of (1-2):2:(1-2).

[0008] Preferably, in T2, the ultrasonic frequency is 20-30 kHz, and the power is 150-200 W; the programmed cooling includes a first stage of reducing from 60-70℃ to 45℃ at a rate of 1.0℃ / min-1.5℃ / min and maintaining for 30-40 min, and a second stage of reducing from 45℃ to 18-24℃ at a rate of 0.2℃ / min-0.5℃ / min.

[0009] Preferably, in T3, the pre-polycondensation conditions are: under a CO2 atmosphere, the pressure is 0.5-0.8 MPa, the temperature is 200-220℃, and the reaction time is 1-1.5 h; the pressure relief polycondensation is relieved to normal pressure at a rate of 0.8 MPa / h, while the temperature is increased to 250-280℃, and the CO2 pressure is maintained at 0.3 MPa for 30-40 min; the vacuum polycondensation is carried out at -0.099 MPa for 40-50 min.

[0010] Preferably, in S3, the setting temperature is 160-185℃, and the time is 30-60 s.

[0011] The application also provides a bio-based synthetic fiber prepared by the preparation method.

[0012] The application also provides a textile product comprising the bio-based synthetic fiber and wool blended fabric.

[0013] Preferably, the textile product is an outdoor sports garment, a casual woven shirt or a sock product.

[0014] Compared with the prior art, the present application has the following advantages and technical effects: The application discloses a kind of bio-based synthetic fiber and wool blended fabric and preparation method thereof, and the blended fabric prepared has the warm and moisture absorption characteristics of wool and the biodegradability of bio-based fiber, the anti-pilling property of the fabric reaches 4-5 levels, the crease recovery angle is greater than or equal to 319 °, the lastingness of pleat is 4-5 levels, the weft elastic elongation is 9.8%-10.7%, the weft non-recovery elongation is 0.4%-0.5%, the appearance grade is excellent, and completely meets the requirements of durability, elasticity and appearance in outdoor sports clothing, casual woven shirts, sock products and other scenes.

[0015] The technical solutions of the present application will be further described in detail below through examples. DETAILED DESCRIPTION

[0016] The technical solutions of the present application will be further described in detail below through examples.

[0017] Unless otherwise defined, the technical terms or scientific terms used in the present application shall have the usual meaning understood by those skilled in the art to which the present application belongs.

[0018] In the present application, unless otherwise specified, other test materials and instruments and equipment are conventional test materials in the art, which can be purchased through commercial channels.

[0019] Example 1 The preparation method of bio-based synthetic fiber comprises the following steps: T1, dry 1 kg of corn straw, crush, pass through a 60 mesh sieve, add 10 L of 1% mass fraction dilute sulfuric acid solution, treat at 121 ℃ for 30 min, cool, filter, wash with water until neutral, collect the solid residue, add distilled water, adjust the substrate concentration to 15% (w / v), simultaneously inoculate 3% by weight of a composite microbial inoculant (the ratio of live yeast bacteria and bacillus is 2:1) and 0.3% by weight of a composite cell wall degrading enzyme (the mass ratio of cellulase, pectinase and xylanase is 1:2:1), ferment at 37 ℃ for 36 h to obtain a fermentation product.

[0020] After the fermentation is completed, the fermentation broth is centrifuged at 10,000 rpm for 10 min at 4 ℃, the supernatant is treated by a ceramic membrane-nanofiltration combined system (0.1 μm ceramic membrane is used for impurity removal, and a 300 Da nanofiltration membrane is used for concentration), the pH is adjusted to 2.8, and the sample is loaded into a modified cation exchange resin column (001×7 type resin is modified by silanization), the loading flow rate is 3 BV / h, deionized water is used for washing until neutral, then 1.5 mol / L ammonia water solution is used for elution at a flow rate of 1.5 BV / h, and the elution peak is collected to obtain a reactant A.

[0021] T2, in a reaction kettle, the reactant A obtained in T1 was added into the reaction kettle with hexanediamine at a molar ratio of 1:1, pH was 7.0, ethanol-water mixed solvent (volume ratio 3:7) was used as the reaction medium, stirring reaction at 62℃ for 1.5h, after the reaction was completed, 28kHz ultrasonic wave (power 200W) was introduced into the system, and the programmed temperature control was started, in the first stage, the temperature was decreased from 62℃ to 45℃ at a rate of 1.0℃ / min, and kept for 30min, in the second stage, the ultrasonic wave was turned off, and the temperature was decreased from 45℃ to 22℃ at a rate of 0.4℃ / min, and the system was kept still for crystallization for 2.5h, then the Buchner funnel was used for suction filtration, and the crystals were washed with a small amount of ice water for 3 times, the wet crystals were placed in a vacuum drying oven, and dried at 60℃ and -0.095MPa for 12h to obtain the reactant B.

[0022] T3, 500g of the reactant B and 0.5g of antioxidant (Irganox 1098) were weighed, 200mL of deionized water was added to prepare a 55wt% aqueous solution, which was added into a polymerization kettle, the kettle was replaced with nitrogen for 3 times, CO2 was introduced until the pressure reached 0.5MPa, the temperature was increased to 210℃ at a rate of 1.5℃ / min, the pressure was increased to 1.6MPa, and the reaction was carried out under the conditions of constant temperature and pressure for 1h, the pressure was released to normal pressure at a rate of 0.8MPa / h, the temperature was increased to 250℃ synchronously, CO2 was introduced to maintain a pressure of 0.3MPa, and the reaction was carried out for 30min, after the pressure release was completed, the vacuum system was started, and the reaction was carried out at -0.099MPa for 40min to obtain the reactant C; T4, the reactant C was first dried in a vacuum drying oven at 80℃ and -0.095MPa for 4h, and then the temperature was increased to 100℃ and -0.099MPa for 5h, after drying, the material was subjected to a twin-screw extruder, the screw zone temperature was set as follows: zone 1 230℃, zone 2 245℃, zone 3 250℃, the metering pump and spinning box temperature was 255℃, the spinning speed was 2800m / min, and a 15kV electrostatic field was applied, the melt stream was cooled and solidified under the condition of ring blowing, the ring blowing temperature was 22℃, the humidity was 70%, the wind speed was 0.8m / s, a liquid nitrogen mist nozzle (mist droplet diameter 5μm) was arranged at a distance of 30cm from the spinning head, after uniform oiling by the oiling wheel, the pre-oriented yarn was wound at a high speed of 3000m / min, and the hot stretching was carried out on a stretching and twisting machine, the first hot roller temperature was 70℃, the second hot roller temperature was 170℃, the stretching multiple was 1.5 times, and the stretching speed was 600m / min to obtain the bio-based synthetic fiber.

[0023] Example 2 The preparation method was the same as that in Example 1, except that in T2, the ultrasonic wave frequency was 20kHz, the power was 150W, and the programmed temperature control included the first stage of decreasing the temperature from 70℃ to 45℃ at a rate of 1.5℃ / min and keeping for 40min, and the second stage of decreasing the temperature from 45℃ to 24℃ at a rate of 0.2℃ / min.

[0024] Example 3 The preparation method is the same as that in Example 1, except that in T3, the precondensation conditions are as follows: under CO2 atmosphere, pressure 0.5 MPa, temperature 220℃, reaction time 1.5 h; the pressure relief condensation is relieved to normal pressure at a rate of 0.8 MPa / h, while the temperature is raised to 280℃, and the CO2 pressure is maintained at 0.3 MPa for 30 min; and the vacuum condensation is carried out at -0.099 MPa for 50 min.

[0025] Example 4 A method for preparing a blended fabric of a bio-based synthetic fiber and wool, comprising the following steps: S1, preparation of blended yarn: wool fibers and bio-based synthetic fibers prepared in Example 1 are mixed in a mass ratio of 3:7, fully opened by an opener, then carded into slivers by a carding machine, and then subjected to two drawing, roving, and ring spinning (twist 700 twists per meter) processes to prepare a 40 English blended yarn; S2, the blended yarn prepared in S1 is used as weft yarn and interwoven with 40 English pure cotton warp yarn on a rapier loom in 2 / 1 twill weave, with the warp density set to 280 ends per 10 cm and the weft density set to 240 ends per 10 cm, to weave into a grey cloth; S3, the grey cloth obtained in S2 is washed in a double-tank fulling machine, with a temperature of 45℃, non-ionic detergent is added, and the washing time is 20 min, then rinsed clean with clean water, and fulling is carried out in an N044 light fulling machine, using an alkaline fulling process (the fulling agent is a mixed solution of neutral soap flakes with a concentration of 30 g / L and pure alkali with a concentration of 15 g / L, and the bath ratio is 1:6), and the specific process parameters are as follows: adjust the pH value to 9.5, treat at 38℃ for 45 min, set the fulling machine pressure to 0.3 MPa, the cloth speed to 14 meters per minute, and use forward and reverse rotation alternately, after treatment, the radial shrinkage of the grey cloth is measured to be 10.5%, and the weft shrinkage is 6.5%, after rinsing with warm water to neutral, and setting at 170℃ for 45 s, the finishing process is completed, to obtain a blended fabric.

[0026] Example 5 The preparation method is the same as that in Example 4, except that the raw material is the bio-based synthetic fiber prepared in Example 2.

[0027] Example 6 The preparation method is the same as that in Example 4, except that the raw material is the bio-based synthetic fiber prepared in Example 3.

[0028] Comparative Example 1 The preparation method is the same as that in Example 1, except that in T1, only yeast is inoculated, without enzyme hydrolysis.

[0029] Comparative Example 2 The preparation method is the same as that in Example 1, except that in T1, only 0.3% by weight of the complex cell wall degrading enzyme is added for enzymolysis.

[0030] Comparative Example 3 The preparation method is the same as that in Example 1, except that in T2, the reactant A obtained in T1 and hexanediamine are added into a reaction kettle at a molar ratio of 1:1, the pH is 7.0, water is used as the reaction medium, stirring is carried out at 62℃ for 1.5h, after the reaction is completed, crystallization is carried out for 2.5h, suction filtration is carried out through a Buchner funnel, the crystal is washed with a small amount of ice water for 3 times, the wet crystal is placed in a vacuum drying box, and drying is carried out at 60℃ and-0.095MPa for 12h to obtain the reactant B.

[0031] Comparative Example 4 The preparation method is the same as that in Example 4, except that the raw material is the bio-based synthetic fiber prepared in Comparative Example 1.

[0032] Comparative Example 5 The preparation method is the same as that in Example 4, except that the raw material is the bio-based synthetic fiber prepared in Comparative Example 2.

[0033] Comparative Example 6 The preparation method is the same as that in Example 4, except that the raw material is the bio-based synthetic fiber prepared in Comparative Example 3.

[0034] The blended fabric prepared in the above Examples 4-6 and Comparative Examples 4-6 is subjected to effect verification.

[0035] The pilling test refers to GB / T 4802.1-2008 “Determination of the Pilling Behavior of Textile - Part 1: Using the Cylinder Method”; the crease recovery angle test refers to GB / T 3819-1997 “Determination of the Crease Recovery of Textile - Part 1: Recovery Angle Method”; the pleat durability test refers to FZ / T 20022-2010 “Textile - Test Methods for Pleat Durability”; the weft elastic elongation and weft non-recovery elongation test both refer to FZ / T 70005-2006 “Textile - Test Methods for Elongation and Recovery”; and the appearance detection refers to GB / T 26382-2011 “Woolen Fabrics”.

[0036] The fabric performance test results are shown in Table 1.

[0037] Table 1: Fabric performance test results

[0038] As shown in Table 1, the fabric provided in Examples 4-6 has a pilling resistance of 4-5 levels, which is much higher than the 2-3 levels of the comparative examples, the fabric provided in the application has significantly improved durability and excellent elastic recovery capacity, and the product appearance quality meets the standard requirements.

[0039] It should be pointed out finally that the above embodiments are only used to illustrate the technical solutions of the present application but not to limit it, and although the present application has been described in detail with reference to the preferred embodiments, it should be understood by those skilled in the art that the technical solutions of the present application can still be modified or replaced equivalently, and these modifications or equivalent replacements should not make the modified technical solutions deviate from the spirit and scope of the technical solutions of the present application.

Claims

1. A process for the production of a blended fabric of bio-based synthetic fibers and wool, characterized in that, It comprises the following steps: S1, mixing wool fibers and bio-based synthetic fibers, and sequentially going through the processes of opening, carding, drawing, roving, and spinning to make blended yarns; S2, weaving the blended yarns prepared in S1 into greige fabrics through the process of shuttle weaving; S3, obtaining blended fabrics after the greige fabrics obtained in S2 go through the processes of scouring, milling, and setting.

2. The preparation method according to claim 1, characterized in that, In S1, the mass ratio of the wool fibers to the bio-based synthetic fibers is (3-7):(2-8).

3. The preparation method according to claim 1, characterized in that, The preparation process of the bio-based synthetic fibers comprises the following steps: T1, after corn stalks are dried, crushed, and pretreated with acid, the corn stalks are inoculated with a compound microbial agent and a compound cell wall degrading enzyme for fermentation, the fermentation liquor is centrifuged, membrane separated, and ion exchanged to obtain a reaction product A; T2, the reaction product A obtained in step T1 is reacted with hexanediamine in an ethanol-water mixed solvent, after the reaction, ultrasonic assisted programmed cooling crystallization is adopted, and after filtration and drying, a reaction product B is obtained; T3, the reaction product B obtained in step T2 is prepared into an aqueous solution, and a pressurized polycondensation reaction is carried out under a CO2 atmosphere, including three stages of pre-polycondensation, pressure relief polycondensation, and vacuum polycondensation, to obtain a reaction product C; T4, after the reaction product C obtained in step T3 is dried, melt spinning is carried out, and an electrostatic field and liquid nitrogen micro-mist quenching are applied synchronously during the spinning process, and after oiling, winding, and heat stretching, a bio-based synthetic fiber is obtained.

4. The preparation method according to claim 3, characterized in that, In T1, the compound microbial agent is composed of yeast and bacillus, and the ratio of the number of viable bacteria is (1-2):1; the compound cell wall degrading enzyme is composed of cellulase, pectinase, and xylanase in a mass ratio of (1-2):2:(1-2).

5. The preparation method according to claim 3, characterized in that, In T2, the ultrasonic frequency is 20-30 kHz, and the power is 150-200 W; the programmed cooling includes a first stage of decreasing from 60-70℃ to 45℃ at a rate of 1.0℃ / min-1.5℃ / min and maintaining for 30-40 min, and a second stage of decreasing from 45℃ to 18-24℃ at a rate of 0.2℃ / min-0.5℃ / min.

6. The preparation method according to claim 3, characterized in that, In T3, the pre-polycondensation conditions are: under a CO2 atmosphere, the pressure is 0.5-0.8 MPa, the temperature is 200-220℃, and the reaction time is 1-1.5 h; the pressure relief polycondensation is relieved to normal pressure at a rate of 0.8 MPa / h, while the temperature is increased to 250-280℃, and the CO2 pressure is maintained at 0.3 MPa for 30-40 min; the vacuum polycondensation is carried out at -0.099 MPa for 40-50 min.

7. The method of claim 1, wherein the step of forming the first and second layers is performed by a process selected from the group consisting of: sputtering, evaporation, and chemical vapor deposition. In S3, the setting temperature is 160-185℃, and the time is 30-60 s.

8. A blended fabric of the bio-based synthetic fiber prepared by the preparation method of claim 1 and wool.

9. A textile, characterized in that, A blended fabric of the bio-based synthetic fiber of claim 8 and wool.

10. The textile of claim 9, wherein, The textile product is an outdoor sports garment, a casual woven shirt, or a hosiery product.

Citation Information

Patent Citations

  • Magnetic graphene oxide surfactant and preparation method thereof

    CN114574238A