Methods for preparing multifunctional plant-based composites for fiber spinning

Abstract

The present invention provides a method for preparing a multifunctional plant-source composite material for fiber spinning, comprising the steps of preparing a modified plant-source powder, preparing a modified nanosilica, preparing a modified polymer matrix, and modifying co-mixing. The intermolecular force between the modified polymer matrix and the modified plant-source powder is stronger. As a result, the adhesion of the active substances in the plant-source powder to the polybutylene succinate is strengthened, and the loss during the preparation and spinning process of the composite material is reduced, while the thermal stability and acid-alkali resistance of the composite material are improved to a certain extent. As a result, the prepared composite material is applicable to the spinning process of multiple types of fibers such as polyester, nylon, acrylic, polypropylene, spandex, lyocell, modal, acetate fiber, viscose fiber, cupra fiber, etc.

Description

[Technical field]

[0001] The present invention relates to the technical field of polymer composites, and in particular to a method for making multifunctional plant-based composites for fiber spinning. [Background technology]

[0002] Fibers are classified into two types: natural fibers and synthetic fibers. Natural fibers have the advantages of moisture absorption, breathability, and comfort, while synthetic fibers have the advantages of strong abrasion resistance, smooth fabric, and resistance to deformation. With the improvement of people's living standards and changes in concepts, the demand for health care functions of fibers is increasing, and the concept of green and environmental protection is also attracting attention. In addition, plants are low-cost, safe and environmentally friendly, so many companies add plant extracts to fibers to give them natural functionality.

[0003] The Chinese patent with the patent number "CN201710846179.6" and the invention title "Plant-sourced bicomponent colored polyester fiber with different melting points and antibacterial function and its preparation method" provides a plant-sourced polyester fiber by adding plant extracts to the polyester fiber. However, during the mixing and extrusion of polyester chips and plant extracts, the temperature is too high, so a large amount of plant extracts are inactivated and the plant active ingredients are lost, resulting in high production costs.

[0004] A Chinese patent with the patent number "CN201310140966.0" and the invention title "Viscose fiber with antibacterial function and fragrance of plant origin and preparation method thereof" describes the addition of plant-origin antibacterial agent and fragrance to viscose fiber. The plant-origin antibacterial agent is a mixed powder of peppermint extract and Isatis root extract, and the fragrance is peppermint oil coated with microcapsules. However, the particle size of the extract is too small, so it is easy to cause aggregation and precipitation in the spinning dope, so if the extract is added directly to the fiber, the mechanical performance of the fiber will be affected to a certain extent. Summary of the Invention [Problem to be solved by the invention]

[0005] In order to solve the problems existing in the prior art, the present invention provides a method for preparing a multifunctional plant-sourced composite material for fiber spinning, and achieves the following objectives of the invention:

[0006] 1. Solve the problem of large amounts of plant-sourced active substances being lost during fiber spinning, and avoid the phenomenon that small-sized plant active granules are prone to agglomeration and uneven distribution in the load matrix;

[0007] 2. To create a multifunctional plant-based composite material with excellent thermal stability, acid and alkali resistance, suitable for various fiber spinning processes, wide range of uses, and industrial-level mass production, sales and promotion.

[0008] 3. To prepare multifunctional plant-sourced composites that have excellent adhesion effect on various kinds of fiber matrices, reduce the loss of plant-sourced active ingredients, endow the fibers with natural and sustained biological activity, and improve the mechanical performance of the fibers. [Means for solving the problem]

[0009] In order to solve the above problems, the present invention employs the following technical solutions.

[0010] A method for preparing a multifunctional plant-sourced composite material for fiber spinning, comprising the steps of preparing a modified plant-source powder S1, preparing a modified nanosilica S2, preparing a modified polymer matrix S3, and performing a modified co-mixing S4. S1. Preparation of modified plant source powder S11. The plant source powder with a particle size of 50-100 nm is placed in anhydrous ethanol, stirred thoroughly for 10-20 minutes, filtered, and the filtrate is collected to obtain the plant source solution;

[0011] S12. Add an interface modifier to the plant source solution described in S11, and ultrasonicate it at 150-200W and 20-40℃ for 5-15min, then adjust the pH to 7.5-8.5, increase the temperature to 50-60℃ and react for 10-20min, cool to room temperature, evaporate anhydrous ethanol, and thoroughly dry at 55-75℃ to obtain the modified plant source powder. However, the plant source powder described in S11 is a plant extract, and the specific type is not limited and can be applied to this system.

[0012] Preferably, the interfacial modifier described in S12 is γ-aminopropyltriethoxysilane and 3-(2,3-epoxypropyl)propyltrioxysilane in a mass ratio of (1.5-2.5):(0.2-0.8), and the amount of the interfacial modifier added is 0.5%-1% of the mass of the plant source powder. S2: Preparation of modified nanosilica

[0013] S21: Add nano-silica to N-methylpyrrolidone under the condition of 50-60℃, and ultrasonically disperse it for 20-30min at an ultrasonic frequency of 80-100kHz. Add silicon-containing unsaturated modifier and stabilizing assistant, react for 10-20h, and then obtain intermediate through centrifugation, ethanol washing, and vacuum drying.

[0014] S22: The intermediate described in S21 is placed in distilled water, ultrasonicated at 100-120 kHz for 15-25 min, and then ethylene glycol dimethacrylate is added under nitrogen protection, the temperature is increased to 80-100°C, and peroxybenzoic acid tert-butyl ester is added and reacted for 2-6 h. The modified nanosilica is obtained through centrifugation, washing with water, and drying.

[0015] Preferably, the mass ratio of the nanosilica described in S21 to the silicon-containing unsaturated modifier and the stabilizing aid is (90-120):(0.5-1.5):(0.01-0.05).

[0016] Furthermore, the silicon-containing unsaturated modifier is a mixture of vinyltris(β-methoxyethoxy)silane and γ-methacryloyloxypropyltrimethoxysilane in a mass ratio of (0.4-1.2):(1.5-2).

[0017] Additionally, the stabilization aid may include one or more combinations of 2,6-di-tert-butyl-p-cresol, p-hydroxyanisole, and 1,1-diphenyl-2-trinitrophenylhydrazine.

[0018] Preferably, the mass ratio of the intermediate described in S22 to ethylene glycol dimethacrylate to tert-butyl peroxybenzoate is (60-80):(90-100):(1-2). S3: Preparation of modified polymer matrix

[0019] The mixture of polyethylene glycol, cationic starch and modified nano-silica is added to polybutylene succinate, and mixed thoroughly at 1500~2500r / min, and then melted and mixed in a mixer to obtain the modified polymer matrix.

[0020] Preferably, the mass ratio of polybutylene succinate, polyethylene glycol, cationic starch, and modified nanosilica described in S3 is (40-50):(10-20):(4-8):(1-5).

[0021] Preferably, the polyethylene glycol described in S3 has a hydroxyl value of 170 to 208 mgKOH / g and a molecular weight of 540 to 660, and the melting and co-mixing temperature is 180 to 200°C. S4: Modified joint mixing

[0022] The modified plant source powder described in S12 and the modified polymer matrix described in S3 are mixed together in a ratio under the condition of a rotation speed of 550-750 r / min, the temperature is slowly increased to 110-120°C at a speed of 4-8°C / min, and reacted for 6-10 hours. Then, a dry modified auxiliary is added, the temperature is continued to be increased to 130-140°C, and melt-mixed together for 10-20 minutes, extruded, and cooled to obtain the multifunctional plant source composite material for fiber spinning.

[0023] Preferably, the amount of the modified plant source powder described in S4 added is 4-12% of the mass of the modified polymer matrix, the mass ratio of the modified polymer matrix to the modifying auxiliary is (4-8):(2-6), and the modifying auxiliary is a mixture of microcrystalline cellulose and polyhydroxybutyrate in a mass ratio of (2-4):(0.5-1.5).

[0024] The multifunctional plant-based composite material is applicable to the spinning process of polyester, nylon, acrylic, polypropylene, spandex, lyocell, modal, acetate fiber, viscose fiber, cupra fiber, etc. Effect of the Invention

[0025] By adopting the above technical solution, the present invention has achieved the following technical effects:

[0026] 1. In the present invention, the modified plant source powder is modified with γ-aminopropyltriethoxysilane and 3-(2,3-epoxypropyl)propyltrioxysilane in a mass ratio of (1.5-2.5):(0.2-0.8), thereby improving the interface performance between the small particle size plant source powder and the polymer matrix, improving the dispersion uniformity of the plant source powder in polybutylene succinate, and reducing the phenomenon that the small particle size plant active granules are easily agglomerated and unevenly dispersed in the load matrix.

[0027] 2. Adding nanosilica to silicon-containing unsaturated modifier can improve the interface performance of nanosilica by interacting with silicon-containing unsaturated modifier and silanol on the surface of nanosilica. In addition, adding stabilizing additive can make the modification proceed more stably and avoid the cross-linking between silicon-containing unsaturated modifier, which affects the progress of modification reaction to some extent. Adding ethylene glycol dimethacrylate and peroxybenzoic acid tert-butyl ester to the intermediate, one end of silicon-containing unsaturated modifier is connected to nanosilica and the other end is connected to ethylene glycol dimethacrylate, and the surface of nanosilica is coated with ethylene glycol dimethacrylate, completing the modification to nanosilica.

[0028] 3. In the present invention, the intermolecular force between the modified polymer matrix and the modified plant-source powder is stronger. As a result, the adhesion of the active ingredients in the plant-source powder to the polybutylene succinate is strengthened, and the loss during the composite preparation and spinning process is reduced. According to the test, the loss rate of the plant-source active ingredients is less than 3%, while the thermal stability and acid-alkali resistance of the composite material are improved to a certain extent. As a result, the prepared composite material can be applied to the spinning process of multiple types of fibers such as polyester, nylon, acrylic, polypropylene, spandex, lyocell, modal, acetate fiber, viscose fiber, and cupra fiber. The addition of this composite material to the above-mentioned fiber provides excellent antibacterial effects, with the antibacterial rates against Staphylococcus aureus, Candida albicans, and Escherichia coli all exceeding 95% (tested according to "GB / T20944.3-2008 vibration method"); the antibacterial loss rate after 100 washings is less than 1% (average value); excellent anti-mite effects, with the anti-mite rate increasing to 99% (tested according to "GB / T24253-2009 Textile Anti-mite Performance Evaluation"); the anti-mite loss rate after 100 washings is less than 2% (average value); good antistatic effects, with the surface resistivity all exceeding 1×10 9The electrical conductivity is less than Ω·cm (tested according to GB / T24249-2009 Antistatic Clean Fabrics). By adding the modification assistant, the modified plant-based powder can be attached more uniformly to the modified polymer matrix and the plasticity of the composite material can be improved. By adding it to the fiber matrix, the compatibility with the fiber is improved, improving the mechanical performance of the fiber.

[0029] 4. The multifunctional plant-based composite material prepared by the present invention can improve the strength, degradability, antibacterial, anti-mite, antistatic and other effects of chemical fibers, and can further enhance the action of various dyes on the fiber surface, improve the dyeability of chemical fibers, and reduce the dyeing temperature of fibers, and can achieve excellent dyeing effect for polyester and nylon at 20-40°C. DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS

[0030] The present invention will now be further described with reference to specific examples. Example 1. Method for preparing multifunctional plant-based composite materials for fiber spinning

[0031] The method for preparing a multifunctional plant-source composite material for fiber spinning includes the steps of preparing modified plant-source powder S1, preparing modified nanosilica S2, preparing modified polymer matrix S3, and modifying co-mixing S4. S1. Preparation of modified plant source powder S11. The plant source powder with a particle size of 100 nm is placed in anhydrous ethanol and stirred thoroughly for 20 minutes, then filtered, and the filtrate is collected to obtain the plant source solution;

[0032] S12. Add an interface modifier to the plant source solution described in S11, and ultrasonicate at 200W and 40°C for 5-15min, then adjust the pH to 8.5, increase the temperature to 60°C and react for 20min, cool to room temperature, evaporate anhydrous ethanol, and thoroughly dry at 75°C to obtain the modified plant source powder. The plant source powder described in S11 is a mixture of green tea extract, honeysuckle extract, peppermint extract and seaweed extract.

[0033] However, the interfacial modifier described in S12 is γ-aminopropyltriethoxysilane and 3-(2,3-epoxypropyl)propyltrioxysilane in a mass ratio of 2.5:0.8, and the amount of the interfacial modifier added is 1% of the mass of the plant source powder. S2: Preparation of modified nanosilica

[0034] S21: Under the condition of 60℃, nano-silica is added to N-methylpyrrolidone, and ultrasonically dispersed for 30 minutes at an ultrasonic frequency of 100kHz. Silicon-containing unsaturated modifier and stabilizing agent are further added, and the mixture is reacted for 20 hours. After that, the intermediate is obtained through centrifugation, ethanol washing, and vacuum drying.

[0035] S22: The intermediate described in S21 is placed in distilled water, ultrasonicated at 120 kHz for 25 min, and then ethylene glycol dimethacrylate is added under nitrogen protection, the temperature is raised to 100°C, and peroxybenzoic acid tert-butyl ester is added and reacted for 6 h. The modified nanosilica is obtained through centrifugation, washing with water, and drying. The mass ratio of nanosilica to silicon-containing unsaturated modifier to stabilizing aid described in S21 is 120:1.5:0.05.

[0036] The silicon-containing unsaturated modifier is a mixture of vinyltris(β-methoxyethoxy)silane and γ-methacryloyloxypropyltrimethoxysilane in a weight ratio of 1.2:2.

[0037] The stabilizing aid comprises 2,6-di-tert-butyl-p-cresol and p-hydroxyanisole in a weight ratio of 1:1. The mass ratio of the intermediate described in S22 to ethylene glycol dimethacrylate to peroxybenzoic acid tert-butyl ester is 80:100:2. S3: Preparation of modified polymer matrix

[0038] The mixture of polyethylene glycol, cationic starch and modified nano-silica is added to polybutylene succinate, and mixed thoroughly at 2500 r / min. The mixture is then melted and mixed in a mixer to obtain the modified polymer matrix. The mass ratio of polybutylene succinate, polyethylene glycol, cationic starch and modified nanosilica described in S3 is 50:20:8:5. The polyethylene glycol described in S3 has a hydroxyl value of 208 mg KOH / g and a molecular weight of 660, and the melting and co-mixing temperature is 200°C. S4: Modified joint mixing

[0039] The modified plant-based powder described in S12 and the modified polymer matrix described in S3 are mixed together in a ratio under the condition of a rotation speed of 750 r / min, the temperature is slowly increased to 120°C at a speed of 8°C / min, and reacted for 10 hours. Then, dry modified additives are added, the temperature is continued to be increased to 140°C, and melt-mixed together for 20 minutes, extruded, and cooled to obtain the multifunctional plant-based composite material for fiber spinning. The loading of the modified plant source powder is 12% by mass of the modified polymer matrix.

[0040] The mass ratio of the modified polymer matrix to the modified auxiliary described in S4 is 8:6, and the modified auxiliary is a mixture of microcrystalline cellulose and polyhydroxybutyrate in a mass ratio of 4:1.5. Example 2. Method for preparing multifunctional plant-based composite materials for fiber spinning

[0041] The method for preparing a multifunctional plant-source composite material for fiber spinning includes the steps of preparing modified plant-source powder S1, preparing modified nanosilica S2, preparing modified polymer matrix S3, and modifying co-mixing S4. S1. Preparation of modified plant source powder S11. The plant source powder with a particle size of 70 nm is placed in anhydrous ethanol and stirred thoroughly for 15 minutes, then filtered, and the filtrate is collected to obtain the plant source solution;

[0042] S12. Add an interfacial modifier to the plant source solution described in S11, and ultrasonicate at 180W and 30°C for 10min, then adjust the pH to 8, increase the temperature to 55°C for 15min reaction, cool to room temperature, evaporate anhydrous ethanol, and thoroughly dry at 65°C to obtain the modified plant source powder. The plant source powder described in S11 is a mixture of green tea extract, honeysuckle extract, peppermint extract and seaweed extract.

[0043] However, the interfacial modifier described in S12 is γ-aminopropyltriethoxysilane and 3-(2,3-epoxypropyl)propyltrioxysilane in a mass ratio of 2:0.5, and the amount of the interfacial modifier added is 0.8% of the mass of the plant source powder. S2: Preparation of modified nanosilica

[0044] S21: Under the condition of 55℃, nano-silica is added to N-methylpyrrolidone, and ultrasonically dispersed for 25min at an ultrasonic frequency of 90kHz. Silicon-containing unsaturated modifier and stabilizing agent are further added, and the mixture is reacted for 15h. After that, the intermediate is obtained through centrifugation, ethanol washing, and vacuum drying.

[0045] S22: The intermediate described in S21 is placed in distilled water, ultrasonicated at 110 kHz for 20 min, and then ethylene glycol dimethacrylate is added under nitrogen protection, the temperature is raised to 90°C, and peroxybenzoic acid tert-butyl ester is added and reacted for 4 h. The modified nanosilica is obtained through centrifugation, washing with water, and drying. The mass ratio of nanosilica to silicon-containing unsaturated modifier to stabilizing aid described in S21 is 110:1:0.03.

[0046] The silicon-containing unsaturated modifier is a mixture of vinyltris(β-methoxyethoxy)silane and γ-methacryloyloxypropyltrimethoxysilane in a weight ratio of 0.8:1.7. The stabilizing aid comprises p-hydroxyanisole and 1,1-diphenyl-2-trinitrophenylhydrazine in a weight ratio of 1:1. The mass ratio of the intermediate described in S22 to ethylene glycol dimethacrylate to peroxybenzoic acid tert-butyl ester is 70:95:1.5. S3: Preparation of modified polymer matrix

[0047] The mixture of polyethylene glycol, cationic starch and modified nano-silica is added to polybutylene succinate, and mixed thoroughly at 2000 r / min. The mixture is then melted and mixed in a mixer to obtain the modified polymer matrix.

[0048] The mass ratio of polybutylene succinate, polyethylene glycol, cationic starch and modified nanosilica described in S3 is 45:15:6:3. The polyethylene glycol described in S3 has a hydroxyl value of 190 mg KOH / g and a molecular weight of 600, and the melting and co-mixing temperature is 190°C. S4: Modified joint mixing

[0049] The modified plant-based powder described in S12 and the modified polymer matrix described in S3 are mixed together in a ratio under the condition of a rotation speed of 650 r / min, the temperature is slowly increased to 115°C at a speed of 6°C / min, and reacted for 8 hours. Then, dry modified auxiliary is added, the temperature is continued to be increased to 135°C, and melt-mixed together for 15 minutes, extruded, and cooled to obtain the multifunctional plant-based composite material for fiber spinning. The loading amount of the modified plant source powder is 9% by mass of the modified polymer matrix.

[0050] The mass ratio of the modified polymer matrix to the modified auxiliary described in S4 is 6:4, and the modified auxiliary is a mixture of microcrystalline cellulose and polyhydroxybutyrate in a mass ratio of 3:1. Example 3: Method for preparing multifunctional plant-based composite materials for fiber spinning

[0051] The method for preparing a multifunctional plant-source composite material for fiber spinning includes the steps of preparing modified plant-source powder S1, preparing modified nanosilica S2, preparing modified polymer matrix S3, and modifying co-mixing S4. S1. Preparation of modified plant source powder S11. The plant source powder with a particle size of 50 nm is placed in anhydrous ethanol and stirred thoroughly for 10 minutes, then filtered, and the filtrate is collected to obtain the plant source solution;

[0052] S12. Add an interfacial modifier to the plant source solution described in S11, and ultrasonicate at 150W and 20°C for 5min, then adjust the pH to 7.5, increase the temperature to 50°C and react for 10min, cool to room temperature, evaporate anhydrous ethanol, and thoroughly dry at 55°C to obtain the modified plant source powder. The plant source powder described in S11 is a mixture of green tea extract, honeysuckle extract, peppermint extract and seaweed extract.

[0053] However, the interfacial modifier described in S12 is γ-aminopropyltriethoxysilane and 3-(2,3-epoxypropyl)propyltrioxysilane in a mass ratio of 1.5:0.2, and the amount of the interfacial modifier added is 0.5% of the mass of the plant source powder. S2: Preparation of modified nanosilica

[0054] S21: Under the condition of 50℃, nano-silica is added to N-methylpyrrolidone, and ultrasonically dispersed for 20min at an ultrasonic frequency of 80kHz. Silicon-containing unsaturated modifier and stabilizing agent are further added, and the mixture is reacted for 10h. After that, the intermediate is obtained through centrifugation, ethanol washing, and vacuum drying.

[0055] S22: The intermediate described in S21 is placed in distilled water, ultrasonicated at 100 kHz for 15 min, and then ethylene glycol dimethacrylate is added under nitrogen protection, the temperature is raised to 80°C, and peroxybenzoic acid tert-butyl ester is added and reacted for 2 h. The modified nanosilica is obtained through centrifugation, washing with water, and drying. The mass ratio of nanosilica to silicon-containing unsaturated modifier to stabilizing aid described in S21 is 90:0.5:0.01.

[0056] The silicon-containing unsaturated modifier is a mixture of vinyltris(β-methoxyethoxy)silane and γ-methacryloyloxypropyltrimethoxysilane in a weight ratio of 0.4:1.5. The stabilizing aid is 2,6-di-tert-butyl-p-cresol. The mass ratio of the intermediate described in S22 to ethylene glycol dimethacrylate to peroxybenzoic acid tert-butyl ester is 60:90:1. S3: Preparation of modified polymer matrix

[0057] The mixture of polyethylene glycol, cationic starch and modified nano-silica is added to polybutylene succinate, and mixed thoroughly at 1500 r / min. The mixture is then melted and mixed in a mixer to obtain the modified polymer matrix. The mass ratio of polybutylene succinate, polyethylene glycol, cationic starch and modified nanosilica described in S3 is 40:10:4:1. The polyethylene glycol described in S3 has a hydroxyl value of 170 mg KOH / g and a molecular weight of 540, and the melting and co-mixing temperature is 180°C. S4: Modified joint mixing

[0058] The modified plant-based powder described in S12 and the modified polymer matrix described in S3 are mixed together in a ratio under the condition of a rotation speed of 550 r / min, the temperature is slowly increased to 110°C at a speed of 4°C / min, and reacted for 6 hours. Then, dry modified auxiliary is added, the temperature is continued to be increased to 130°C, and melt-mixed together for 10 minutes, extruded, and cooled to obtain the multifunctional plant-based composite material for fiber spinning. The loading amount of the modified plant source powder is 4% of the mass of the modified polymer matrix.

[0059] The mass ratio of the modified polymer matrix to the modified auxiliary described in S4 is 4:2, and the modified auxiliary is a mixture of microcrystalline cellulose and polyhydroxybutyrate in a mass ratio of 2:0.5.

[0060] The multifunctional plant-source composite materials for fiber spinning prepared in Examples 1 to 3 are added to viscose fiber, polyester fiber, and nylon fiber at a loading amount of 3% to measure their performance. Specifically, see Tables 1, 2, and 3.

[0061] Table 1 JPEG0007689393000001.jpg65170

[0062] Table 2 JPEG0007689393000002.jpg59170

[0063] Table 3 JPEG0007689393000003.jpg59170

[0064] Measurement Standard Mechanical properties: GB / T3923.1-2013 Test methods for tensile properties, breaking strength and breaking elongation of textiles and woven fabrics. Dyeing uniformity: Measure the level of the gray card according to "Testing and evaluation of dyeing uniformity of viscose filament (FZ / T50015-2009)". Color fastness to washing: "GB-T / 3921-2008 Color fastness test of textile fabrics, color fastness to soap washing". Antibacterial rate: "GB / T20944.3-2008 vibration method". Mite prevention rate: "GB / T24253-2009 Evaluation of anti-mite performance of textile fabrics". Surface resistivity: GB / T24249-2009 Antistatic clean fabrics.

[0065] As can be seen from the table, by adding the multifunctional plant-based composite materials for fiber spinning prepared in Examples 1 to 3 to viscose fiber, polyester fiber, and nylon fiber, the mechanical properties of the fibers are excellent, the loss rate of plant-based active ingredients during the spinning process is low, the dyeing performance and color fastness to washing of the fibers are good, and the antibacterial rate is good, with the antibacterial rates against Staphylococcus aureus, Candida albicans, and Escherichia coli all being 95% or more, and the antibacterial loss rate after 100 water washes is less than 1% (average value), the anti-mite effect is excellent, with the mite prevention rate being up to 99%, and the mite prevention loss rate after 100 water washes is less than 2% (average value), and the antistatic effect is good, with the surface resistivity being 1×10 9 It is less than Ω·cm.

[0066] As can be seen from the above, the multifunctional plant-based composite material prepared in the present invention has good thermal stability and acid and alkali resistance, reduces the loss of plant-based active ingredients during the composite material preparation process and spinning process, strengthens chemical fibers to a certain extent to provide fiber functionality, further enhances the activity of various dyes on the fiber surface, improves the dyeability of chemical fibers, and can reduce the fiber dyeing temperature, and can achieve excellent dyeing effect on polyester and nylon at 20-40°C. Comparative Example 1

[0067] Select the representative Example 2, and use γ-aminopropyltriethoxysilane and 3-(2,3-epoxypropyl)propyltrioxysilane with mass ratios of 3:0.1 and 0.1:3, respectively, to modify the modified plant source powder, and the rest are consistent with Example 2. During the modification co-mixing, the modified plant source powder obtained in Comparative Example 1 still generates the phenomenon of aggregation and non-uniform dispersion in the modified polymer matrix. Comparative Example 2

[0068] Select the representative Example 2, add the amount of interfacial modifier as 0, and other are consistent with Example 2. In Comparative Example 2, when other preparation processes are not changed, the phenomenon of aggregation and non-uniform dispersion also occurs during the process of co-mixing the plant source powder with the polymer matrix. As can be seen, the interfacial modifier improves the mixing performance of the plant source powder and the polymer matrix, makes the mixture of the modified plant source powder with the whole polymer more uniform, and makes the quality of the final product more stable. Comparative Example 3

[0069] Select the representative Example 2, remove the preparation step of the polymer matrix, directly modify and co-mix the modified plant source powder with polybutylene succinate, and otherwise match the Example 2. As the comparative example 3, add the prepared composite material to viscose fiber, polyester fiber, and nylon fiber at a 3% addition amount, respectively, to measure their performance. Specifically, refer to Table 4.

[0070] Table 4 JPEG0007689393000004.jpg36170

[0071] It can be seen that the intermolecular force between the modified polymer matrix and the modified plant-based powder is stronger, which strengthens the adhesion of the active substances in the plant-based powder to the polybutylene succinate, reducing the loss during the composite fabrication and spinning process, while improving the thermal stability and acid-alkali resistance of the composite to a certain extent, and improving the mechanical properties and dyeing performance of the fiber. Comparative Example 4

[0072] Select a representative Example 2, remove the modification aid step, and otherwise match with Example 2. As Comparative Example 4, add the prepared composite material to viscose fiber, polyester fiber, and nylon fiber at a loading amount of 3% to measure their mechanical properties. Specifically, refer to Table 5.

[0073] Table 5 JPEG0007689393000005.jpg29170

[0074] The addition of the modification aid allows the modified plant-source powder to adhere more uniformly to the modified polymer matrix and improves the plasticity of the composite material. By adding the modification aid to the fiber matrix, it improves the compatibility with the fiber, thereby improving the mechanical performance of the fiber. The ratios described in the present invention are all mass ratios unless otherwise specified, and the percentages mentioned above are mass percentages, and all raw materials are purchased from the market.

[0075] Finally, the above is only a preferred embodiment of the present invention, and is not intended to limit the present invention, and the present invention has been described in detail with reference to the above embodiment, but those skilled in the art may still modify the technical solutions described in the above embodiment or replace some of the technical features with equivalents. Any modifications, equivalent replacements, improvements, etc. made within the spirit and principle of the present invention are all included in the protection scope of the present invention.

Claims

1. A method for making a multifunctional plant-sourced composite material for fiber spinning, comprising: The method includes the steps of preparing a modified plant source powder, preparing a modified nanosilica, preparing a modified polymer matrix, and modifying the co-mixing step; The step of preparing the modified plant source powder comprises: stirring the plant source powder in absolute ethanol, followed by filtering and collecting the filtrate to obtain a plant source solution; and modifying the plant source solution by adding an interfacial modifier to obtain a modified plant source powder; The step of preparing the modified nanosilica comprises: Add nanosilica to N-methylpyrrolidone at 50-60°C, ultrasonically disperse the mixture at an ultrasonic frequency of 80-100kHz for 20-30min, add a silicon-containing unsaturated modifier and a stabilizing aid, react for 10-20h, and then centrifuge, wash with ethanol, and vacuum dry to obtain an intermediate. The intermediate is subjected to ultrasonic treatment in distilled water at 100-120 kHz for 15-25 min, ethylene glycol dimethacrylate is added in a nitrogen atmosphere, the temperature is raised to 80-100° C., peroxybenzoic acid tert-butyl ester is added, and the reaction is carried out for 2-6 h. Then, the intermediate is centrifuged, washed with water, and dried to obtain a modified nanosilica. The step of preparing the modified polymer matrix comprises: The method includes the steps of adding the mixture of polyethylene glycol, cationic starch and the modified nano-silica to polybutylene succinate, mixing at 1500-2500 r / min, and then melting and co-mixing in a mixer to obtain a modified polymer matrix; The modification co-mixing step comprises: The modified plant-source powder and the modified polymer matrix are mixed together at a rotation speed of 550-750 r / min, and the temperature is increased to 110-120°C at a speed of 4-8°C / min for 6-10 h. Then, a modification assistant is added, the temperature is increased to 130-140°C, and the mixture is melted and mixed together for 10-20 min. The mixture is extruded and cooled to obtain a multifunctional plant-source composite material for fiber spinning. The interfacial modifier is γ-aminopropyltriethoxysilane and 3-(2,3-epoxypropyl)propyltrioxysilane. The mass ratio of the γ-aminopropyltriethoxysilane and the 3-(2,3-epoxypropyl)propyltrioxysilane is 1.5 to 2.5:0.2 to 0.

8. A method for preparing a multifunctional plant-based composite material for fiber spinning, comprising:

2. The modification conditions in the step of preparing the modified plant source powder are: ultrasonic treatment at 20-40°C for 5-15 minutes, pH adjustment to 7.5-8.5, temperature increase to 50-60°C for reaction for 10-20 minutes, cooling to room temperature, evaporating anhydrous ethanol, and drying at 55-75°C. A method for making a multifunctional plant-based composite material for fiber spinning according to claim 1.

3. The amount of the interfacial modifier added in the step of preparing the modified plant source powder is 0.5% to 1% of the mass of the plant source powder; A method for making a multifunctional plant-based composite material for fiber spinning according to claim 1.

4. In the step of preparing the modified nanosilica, the mass ratio of the nanosilica to the silicon-containing unsaturated modifier to the stabilizing aid is 90-120:0.5-1.5:0.01-0.05; The mass ratio of the intermediate to ethylene glycol dimethacrylate to peroxybenzoic acid tert-butyl ester is 60-80:90-100:1-2; A method for making a multifunctional plant-based composite material for fiber spinning according to claim 1.

5. In the step of preparing the modified nanosilica, the silicon-containing unsaturated modifier is a mixture of vinyltris(β-methoxyethoxy)silane and γ-methacryloyloxypropyltrimethoxysilane in a mass ratio of 0.4-1.2:1.5-2; The stabilizing aid includes one or more combinations of 2,6-di-tert-butyl-p-cresol, p-hydroxyanisole, and 1,1-diphenyl-2-trinitrophenylhydrazine; A method for making a multifunctional plant-based composite material for fiber spinning according to claim 1.

6. In the step of preparing the modified polymer matrix, the mass ratio of the polybutylene succinate, the polyethylene glycol, the cationic starch and the modified nanosilica is 40-50: 10-20: 4-8: 1-5; A method for making a multifunctional plant-based composite material for fiber spinning according to claim 1.

7. The amount of the modified plant source powder added in the modified co-mixing step is 4-12% of the mass of the modified polymer matrix; A method for making a multifunctional plant-based composite material for fiber spinning according to claim 1.

8. The mass ratio of the modified polymer matrix to the modified auxiliary in the modified co-mixing step is 4-8:2-6; The modification aid is a mixture of microcrystalline cellulose and polyhydroxybutyrate in a mass ratio of 2-4:0.5-1.5; A method for making a multifunctional plant-based composite material for fiber spinning according to claim 1.

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