A method for preparing bamboo fiber for textiles
By immobilizing pectinase using mesoporous silica, the problem of high enzyme loss rate in biological enzymatic methods was solved, improving the extraction efficiency and quality of bamboo fiber and achieving stable enzyme immobilization and efficient fiber production.
Patent Information
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- ZHEJIANG QINGSHI NEW MATERIAL TECHNOLOGY CO LTD
- Filing Date
- 2026-01-31
- Publication Date
- 2026-05-26
AI Technical Summary
In the existing bio-enzymatic extraction process of bamboo fiber, the enzyme loss rate is high, which leads to a decline in fiber quality and an increase in production costs. Furthermore, the effect of immobilized enzymes is unstable.
Pectinase was immobilized in mesoporous silica. The mesoporous silica was then treated with 3-aminopropyltriethoxysilane and cross-linked with chitosan to form a porous network structure, which improved the enzyme loading and stability and reduced the enzyme residue in the fiber.
It significantly reduced the enzyme loss rate, improved the extraction efficiency and quality of bamboo fiber, maintained the whiteness and mechanical properties of the fiber, and achieved an enzyme activity retention rate of 66.3-68.4%.
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Abstract
Description
Technical Field
[0001] This invention belongs to the field of fiber extraction technology, specifically relating to a method for preparing bamboo fiber for textiles. Background Technology
[0002] Bamboo fiber is a natural cellulose fiber extracted from bamboo, retaining the natural properties of bamboo. Its main uses include: making antibacterial, breathable, and cool clothing and home textile products; using it as a reinforcing material in environmentally friendly composite materials, automotive interiors, and industrial fabrics; and it can also be processed into environmentally friendly packaging materials, disposable hygiene products, and high-value-added paper products. With its advantages of being green, biodegradable, and renewable, it has become a highly regarded eco-friendly material.
[0003] The main methods for extracting bamboo fiber include mechanical, chemical, and bio-enzymatic methods. Among them, the mechanical method directly separates the fiber through mechanical forces such as rolling, combing, and thermal coupling. This method is environmentally friendly (usually without chemical additives), but the fibers are relatively coarse and the separation effect is poor. The chemical method uses chemical reagents such as alkali to cook bamboo chips, softening lignin, etc., and then obtains the fiber through mechanical rolling and combing. This method can effectively destroy lignin, hemicellulose, etc. in bamboo, with good separation effect and significantly improved spinnability. The process is relatively mature, but the production process generates a large amount of wastewater containing alkali (or other chemicals), which poses an environmental pollution risk. Secondly, chemical treatment may cause certain damage to the natural structure and mechanical properties of the fiber, and it involves multiple processes such as cooking and rinsing, resulting in high consumption of water, steam, and chemicals, and high costs.
[0004] As people become more aware of safety, environmental protection, and green practices, the bio-enzymatic extraction of bamboo fiber has become mainstream. The bio-enzymatic method is environmentally friendly, has mild reaction conditions, and produces high-quality fibers. However, the bio-enzymatic method has two drawbacks: 1. After processing, enzymes may remain in the gaps between bamboo strips or be lost during the washing process, with an enzyme loss rate of 15-20%, increasing costs; 2. The residual enzymes may undergo browning during the drying process, leading to a decrease in fiber whiteness.
[0005] Immobilizing enzymes on a carrier can reduce enzyme loss and residue in the gaps of bamboo strips. However, after 3 to 5 uses, the immobilization effect of the carrier on the enzyme decreases significantly, and a large amount of enzyme is lost. Summary of the Invention
[0006] In view of the problems existing in the prior art, the present invention provides a method for preparing bamboo raw fiber for textiles, which achieves the following objectives: improving the immobilization effect of mesoporous silica on enzymes, thereby reducing enzyme loss rate and improving bamboo raw fiber extraction efficiency.
[0007] To solve the above technical problems, the technical solution adopted by the present invention is as follows: A method for preparing bamboo fiber for textile use, comprising: 1. Bamboo strip pretreatment Take whole bamboo, crush and cut it, and take bamboo strips with a length of 6-8cm, a width of 0.5-0.7cm, and a thickness of 0.3-0.5cm. Soak the strips in NaOH solution for 30-40 minutes, filter them, wash them with deionized water until neutral, and dry them until the moisture content is 15-20% to obtain pretreated bamboo strips. The bamboo in question is of the Ci bamboo variety. The ultrasonic frequency is 40–60 kHz. The NaOH solution has a mass fraction of 0.2% to 0.5%.
[0008] 2. Immobilized enzymes S1. Add mesoporous silica to deionized water, then add 3-aminopropyltriethoxysilane, stir for 25-35 min, filter, wash intermediate product A with deionized water, add to phosphate buffer, then add pectinase, centrifuge for 2.5-3.5 h to obtain intermediate product B. S2. Add chitosan and sodium alginate to deionized water, sonicate to remove bubbles, heat to 45-55℃, add sucrose ester, stir and emulsify for 8-12 minutes, then add intermediate product B, continue stirring for 25-35 minutes, slowly add CaCl2 solution, let stand for 25-35 minutes after the addition is complete, filter, wash with deionized water until neutral, and obtain immobilized pectinase. Using the same method, immobilized xylanase and immobilized laccase were prepared by replacing pectinase with equal masses of xylanase and laccase, respectively. In step S1, the mass ratio of mesoporous silica, deionized water, and 3-aminopropyltriethoxysilane is 1.9–2.3:6–8:0.4–0.5. The mesoporous silica has a particle size of 300–500 nm and a pore size of 5–15 nm. The mass ratio of intermediate product A, phosphate buffer, and pectinase is 0.8–1.2:12–14:0.05–0.07. In step S2, the mass ratio of intermediate product B, chitosan, sodium alginate, deionized water, sucrose ester, and CaCl2 solution is 0.4–0.6: 2.2–2.5: 1.4–1.6: 20–25: 0.1–0.2: 5–6. The mass fraction of the CaCl2 solution is 3-5%; The stirring rate is 50–70 r / min; The CaCl2 solution was added dropwise at a rate of 3–5 ml / min.
[0009] 3. Extracting bamboo fiber Pretreated bamboo chips were added to immobilized pectinase buffer and enzymatically hydrolyzed at 45–55°C for 2–3 hours. After filtration, the intermediate product was rinsed with deionized water and then added again to a mixed buffer of immobilized xylanase and immobilized laccase. After enzymatic hydrolysis at 45–55°C for 1–2 hours, the product was filtered, rinsed with deionized water, and dried at 40–50°C for 20–30 minutes to obtain bamboo raw fibers. The bamboo raw fibers were then fed into a carding machine for carding to obtain bamboo raw fibers for textiles. The mass ratio of the pretreated bamboo strips to the immobilized pectinase buffer is 0.9–1.1:28–32; The immobilized pectinase buffer solution contains 3-4% by mass of immobilized pectinase. The mass ratio of the intermediate product, immobilized xylanase, and immobilized laccase in the mixed buffer solution is 0.9–1.1:28–32. In the mixed buffer solution of immobilized xylanase and immobilized laccase, the mass fraction of immobilized xylanase is 1.5-2.1%, and the mass fraction of immobilized laccase is 0.7-0.9%. The bamboo fiber used in textiles has a fineness of 5.5 to 6.5 dtex.
[0010] Compared with the prior art, the beneficial effects of the present invention are as follows: 1. Pre-treat bamboo with ultrasound. The cavitation effect of ultrasound can tear the cell walls of bamboo and increase the porosity. At the same time, soaking in a 0.2-0.5% NaOH solution dissolves some of the surface pectin, reducing the resistance to subsequent enzymatic hydrolysis and improving the efficiency of enzymatic hydrolysis.
[0011] 2. Pectinase is immobilized using mesoporous silica. First, the mesoporous silica is silanized using 3-aminopropyltriethoxysilane to introduce amino groups. Through electrostatic interaction, the negatively charged pectinase is bound, significantly increasing the loading capacity. Then, chitosan is used for mild cross-linking, forming a porous network structure on the surface of the mesoporous silica. This increases mechanical strength and reduces the pore size of the mesoporous silica, thus reducing the loss of pectinase during use.
[0012] 3. Immobilized enzymes are used, making it easier to remove them from the fibers and reducing the residual rate of enzymes in the fibers. At the same time, the washing liquid can be concentrated, recycled, and reused.
[0013] 4. The bamboo fiber extracted by this invention has a tensile strength of 1.21-1.28 GPa, a breaking elongation of 4.09-4.17%, an elastic modulus of 37.15-37.26 GPa, and an average activity retention rate of 66.3-68.4% for the immobilized enzyme after 10 repeated uses. Detailed Implementation
[0014] Example 1 1. Bamboo strip pretreatment Take whole bamboo, crush and cut it, take bamboo strips with a length of 7cm, a width of 0.6cm and a thickness of 0.4cm, ultrasonically treat for 30min, then soak in NaOH solution for 35min, filter, wash with deionized water until neutral, and dry to a moisture content of 18% to obtain pretreated bamboo strips. The bamboo in question is of the Ci bamboo variety. The ultrasonic frequency is 50kHz. The NaOH solution has a mass fraction of 0.3%.
[0015] 2. Immobilized enzymes S1. Add mesoporous silica to deionized water, then add 3-aminopropyltriethoxysilane, stir for 30 min, filter, wash intermediate product A with deionized water, add to phosphate buffer, then add pectinase, centrifuge after 3 h to obtain intermediate product B. S2. Add chitosan and sodium alginate to deionized water, sonicate to remove bubbles, heat to 50°C, add sucrose ester, stir and emulsify for 10 min, then add intermediate product B, continue stirring for 30 min, slowly add CaCl2 solution, let stand for 30 min after the addition is complete, filter, wash with deionized water until neutral, and obtain immobilized pectinase. Using the same method, immobilized xylanase and immobilized laccase were prepared by replacing pectinase with equal masses of xylanase and laccase, respectively. In step S1, the mass ratio of mesoporous silica, deionized water, and 3-aminopropyltriethoxysilane is 2.1:7:0.45. The mesoporous silica has a particle size of 400 nm and a pore size of 10 nm; The mass ratio of intermediate product A, phosphate buffer, and pectinase is 1:13:0.06; In step S2, the mass ratio of intermediate product B, chitosan, sodium alginate, deionized water, sucrose ester, and CaCl2 solution is 0.5:2.3:1.5:23:0.15:5.5. The mass fraction of the CaCl2 solution is 4%; The stirring rate is 60 r / min; The CaCl2 solution was added dropwise at a rate of 4 ml / min.
[0016] 3. Extracting bamboo fiber Pretreated bamboo chips were added to immobilized pectinase buffer and enzymatically hydrolyzed at 50°C for 2.5 h. After filtration, the intermediate product was rinsed with deionized water and then added again to a mixed buffer of immobilized xylanase and immobilized laccase. After enzymatic hydrolysis at 50°C for 1.5 h, the product was filtered, rinsed with deionized water, and dried at 45°C for 25 min to obtain bamboo raw fibers. The bamboo raw fibers were then fed into a carding machine for carding to obtain bamboo raw fibers for textiles. The mass ratio of the pretreated bamboo strips to the immobilized pectinase buffer is 1:30. The immobilized pectinase buffer solution contains 3.5% immobilized pectinase by mass. The mass ratio of the intermediate product, immobilized xylanase, and immobilized laccase in the mixed buffer solution is 1:30. In the mixed buffer solution of immobilized xylanase and immobilized laccase, the mass fraction of immobilized xylanase is 1.8%, and the mass fraction of immobilized laccase is 0.8%. The bamboo fiber used in textiles has a fineness of 6 dtex.
[0017] Example 2 1. Bamboo strip pretreatment Take whole bamboo, crush and cut it, take bamboo strips with a length of 6cm, a width of 0.5cm and a thickness of 0.3cm, ultrasonically treat for 25min, then soak in NaOH solution for 30min, filter, wash with deionized water until neutral, and dry to a moisture content of 15% to obtain pretreated bamboo strips. The bamboo in question is of the Ci bamboo variety. The ultrasonic frequency is 40kHz; The NaOH solution has a mass fraction of 0.2%.
[0018] 2. Immobilized enzymes S1. Add mesoporous silica to deionized water, then add 3-aminopropyltriethoxysilane, stir for 25 min, filter, wash intermediate product A with deionized water, add to phosphate buffer, then add pectinase, centrifuge after 2.5 h to obtain intermediate product B. S2. Add chitosan and sodium alginate to deionized water, sonicate to remove bubbles, heat to 45°C, add sucrose ester, stir and emulsify for 8 minutes, then add intermediate product B, continue stirring for 25 minutes, slowly add CaCl2 solution, let stand for 25 minutes after the addition is complete, filter, wash with deionized water until neutral, and obtain immobilized pectinase. Using the same method, immobilized xylanase and immobilized laccase were prepared by replacing pectinase with equal masses of xylanase and laccase, respectively. In step S1, the mass ratio of mesoporous silica, deionized water, and 3-aminopropyltriethoxysilane is 1.9:6:0.4. The mesoporous silica has a particle size of 300 nm and a pore size of 5 nm. The mass ratio of intermediate product A, phosphate buffer, and pectinase is 0.8:12:0.05; In step S2, the mass ratio of intermediate product B, chitosan, sodium alginate, deionized water, sucrose ester, and CaCl2 solution is 0.4:2.2:1.4:20:0.1:5. The mass fraction of the CaCl2 solution is 3%; The stirring rate is 50 r / min; The CaCl2 solution was added dropwise at a rate of 3 ml / min.
[0019] 3. Extracting bamboo fiber Pretreated bamboo chips were added to immobilized pectinase buffer and enzymatically hydrolyzed at 45°C for 2 hours. After filtration, the intermediate product was rinsed with deionized water and then added to a mixed buffer of immobilized xylanase and immobilized laccase. After enzymatic hydrolysis at 45°C for 1 hour, the product was filtered, rinsed with deionized water, and dried at 40°C for 20 minutes to obtain bamboo raw fibers. The bamboo raw fibers were then fed into a combing machine for combing to obtain bamboo raw fibers for textiles. The mass ratio of the pretreated bamboo strips to the immobilized pectinase buffer was 0.9:28. The immobilized pectinase buffer solution contains 3% immobilized pectinase by mass. The mass ratio of the intermediate product, immobilized xylanase, and immobilized laccase in the mixed buffer solution is 0.9:28. In the mixed buffer solution of immobilized xylanase and immobilized laccase, the mass fraction of immobilized xylanase is 1.5% and the mass fraction of immobilized laccase is 0.7%. The bamboo fiber used in textiles has a fineness of 5.5 dtex.
[0020] Example 3 1. Bamboo strip pretreatment Take whole bamboo, crush and cut it, take bamboo strips with a length of 8cm, a width of 0.7cm and a thickness of 0.5cm, ultrasonically treat for 35min, then soak in NaOH solution for 40min, filter, wash with deionized water until neutral, and dry to a moisture content of 20% to obtain pretreated bamboo strips; The bamboo in question is of the Ci bamboo variety. The ultrasonic frequency is 60kHz. The NaOH solution has a mass fraction of 0.5%.
[0021] 2. Immobilized enzymes S1. Add mesoporous silica to deionized water, then add 3-aminopropyltriethoxysilane, stir for 35 min, filter, wash intermediate product A with deionized water, add to phosphate buffer, then add pectinase, centrifuge after 3.5 h to obtain intermediate product B. S2. Add chitosan and sodium alginate to deionized water, sonicate to remove bubbles, heat to 55°C, add sucrose ester, stir and emulsify for 12 min, then add intermediate product B, continue stirring for 35 min, slowly add CaCl2 solution, let stand for 35 min after the addition is complete, filter, wash with deionized water until neutral, and obtain immobilized pectinase. Using the same method, immobilized xylanase and immobilized laccase were prepared by replacing pectinase with equal masses of xylanase and laccase, respectively. In step S1, the mass ratio of mesoporous silica, deionized water, and 3-aminopropyltriethoxysilane is 2.3:8:0.5. The mesoporous silica has a particle size of 500 nm and a pore size of 15 nm. The mass ratio of intermediate product A, phosphate buffer, and pectinase is 1.2:14:0.07. In step S2, the mass ratio of intermediate product B, chitosan, sodium alginate, deionized water, sucrose ester, and CaCl2 solution is 0.6:2.5:1.6:25:0.2:6. The mass fraction of the CaCl2 solution is 5%; The stirring rate is 70 r / min; The CaCl2 solution was added dropwise at a rate of 5 ml / min.
[0022] 3. Extracting bamboo fiber Pretreated bamboo chips were added to immobilized pectinase buffer and enzymatically hydrolyzed at 45°C for 2 hours. After filtration, the intermediate product was rinsed with deionized water and then added to a mixed buffer of immobilized xylanase and immobilized laccase. After enzymatic hydrolysis at 45°C for 1 hour, the product was filtered, rinsed with deionized water, and dried at 40°C for 20 minutes to obtain bamboo raw fibers. The bamboo raw fibers were then fed into a combing machine for combing to obtain bamboo raw fibers for textiles. The mass ratio of the pretreated bamboo strips to the immobilized pectinase buffer was 0.9:28. The immobilized pectinase buffer solution contains 3% immobilized pectinase by mass. The mass ratio of the intermediate product, immobilized xylanase, and immobilized laccase in the mixed buffer solution is 0.9:28. In the mixed buffer solution of immobilized xylanase and immobilized laccase, the mass fraction of immobilized xylanase is 1.5% and the mass fraction of immobilized laccase is 0.7%. The bamboo fiber used in textiles has a fineness of 6.5 dtex.
[0023] Comparative Example 1 Based on Example 1, the step of immobilizing the enzyme is omitted, and in step 3, an equal mass of enzyme is used to replace the immobilizing enzyme. The remaining steps are the same, specifically: 1. Bamboo strip pretreatment Take whole bamboo, crush and cut it, take bamboo strips with a length of 1.5cm, a width of 0.6cm and a thickness of 0.4cm, treat them with ultrasound for 30min, then soak them in NaOH solution for 35min, filter them, wash them with deionized water until neutral, and dry them until the moisture content is 18% to obtain pretreated bamboo strips. The bamboo in question is of the Ci bamboo variety. The ultrasonic frequency is 50kHz. The NaOH solution has a mass fraction of 0.3%.
[0024] 2. Extraction of bamboo fiber Pretreated bamboo chips were added to pectinase buffer and enzymatically hydrolyzed at 50°C for 2.5 hours. After filtration, the intermediate product was rinsed with deionized water and then added to a mixed buffer of xylanase and laccase. After enzymatic hydrolysis at 50°C for 1.5 hours, the product was filtered, rinsed with deionized water, and dried at 45°C for 25 minutes to obtain bamboo raw fibers. The bamboo raw fibers were then fed into a carding machine for carding to obtain bamboo raw fibers for textile use. The mass ratio of the pretreated bamboo strips to the pectinase buffer is 1:30. The pectinase buffer solution contains 3.5% pectinase by mass. The mass ratio of the intermediate product, xylanase, and laccase in the mixed buffer solution is 1:30. In the mixed buffer solution of xylanase and laccase, the mass fraction of xylanase is 1.8% and the mass fraction of laccase is 0.8%. The bamboo fiber used in textiles has a fineness of 6 dtex.
[0025] Comparative Example 2 Based on Example 1, step S2 in step 2 is omitted, and intermediate product B is used instead of immobilized pectinase. All other steps are the same.
[0026] Test case 1. The bamboo fibers prepared in Examples 1-3 and Comparative Examples 1-2 were tested for tensile strength, elongation at break, elastic modulus, and the average activity retention rate of the immobilized enzyme after 10 repeated uses. The test results are shown in Table 1: Table 1
[0027] 2. Bamboo fibers were prepared 10 times using the methods of Examples 1-3 and Comparative Examples 1-2, respectively. The Gann whiteness values of the bamboo fibers prepared on the 1st, 4th, 7th, and 10th batches were tested. The test results are shown in Table 2.
[0028] As shown in Table 1, Comparative Example 1 did not fix the enzyme, resulting in significant enzyme loss and activity reduction during use. Although Comparative Example 2 fixed the enzyme, it did not use chitosan for cross-linking. The mesoporous silica had a large pore size, which caused some enzyme to detach and be lost during use. With increasing usage, the enzyme fixation effect of the mesoporous silica in Comparative Example 2 gradually decreased, and some enzyme migrated and remained on the bamboo fiber, resulting in a gradual decrease in fiber whiteness.
Claims
1. A method for preparing bamboo fiber for textiles, characterized in that: The preparation method includes bamboo strip pretreatment, enzyme immobilization, and bamboo fiber extraction; The method for pretreating bamboo strips is as follows: take whole bamboo, crush and cut it, take bamboo strips with a length of 6-8cm, a width of 0.5-0.7cm, and a thickness of 0.3-0.5cm, treat them with ultrasound for 25-35min, then soak them in NaOH solution for 30-40min, filter them, wash them with deionized water until neutral, and dry them until the moisture content is 15-20% to obtain pretreated bamboo strips.
2. The method for preparing bamboo fiber for textiles according to claim 1, characterized in that: In the method for pre-treating bamboo strips, the bamboo species is *Phyllostachys edulis*. The ultrasonic frequency is 40–60 kHz; The mass fraction of the NaOH solution is 0.2% to 0.5%.
3. The method for preparing bamboo fiber for textiles according to claim 1, characterized in that: The method for immobilizing the enzyme includes S1 and S2; The method described in S1 is as follows: mesoporous silica is added to deionized water, then 3-aminopropyltriethoxysilane is added, the mixture is stirred for 25-35 minutes, filtered, intermediate product A is washed with deionized water, added to phosphate buffer, then pectinase is added, and after 2.5-3.5 hours, it is centrifuged to obtain intermediate product B.
4. The method for preparing bamboo fiber for textiles according to claim 3, characterized in that: The method of S2 is as follows: chitosan and sodium alginate are added to deionized water, ultrasonically degassing is performed, the temperature is raised to 45-55°C, sucrose ester is added, and emulsification is carried out by stirring for 8-12 minutes. Then intermediate product B is added, and stirring is continued for 25-35 minutes. CaCl2 solution is slowly added dropwise. After the addition is completed, the mixture is allowed to stand for 25-35 minutes, filtered, and washed with deionized water until neutral to obtain immobilized pectinase. Using the same method, immobilized xylanase and immobilized laccase were prepared by replacing pectinase with equal masses of xylanase and laccase, respectively.
5. The method for preparing bamboo fiber for textiles according to claim 3, characterized in that: In the method for immobilizing the enzyme, in step S1, the mass ratio of mesoporous silica, deionized water, and 3-aminopropyltriethoxysilane is 1.9–2.3:6–8:0.4–0.
5. The particle size of mesoporous silica is 300–500 nm, and the pore size is 5–15 nm. The mass ratio of intermediate product A, phosphate buffer, and pectinase is 0.8–1.2:12–14:0.05–0.
07. In step S2, the mass ratio of intermediate product B, chitosan, sodium alginate, deionized water, sucrose ester, and CaCl2 solution is 0.4–0.6: 2.2–2.5: 1.4–1.6: 20–25: 0.1–0.2: 5–6. The mass fraction of CaCl2 solution is 3-5%; The stirring rate is 50–70 r / min; Add CaCl2 solution dropwise at a rate of 3–5 ml / min.
6. The method for preparing bamboo fiber for textiles according to claim 1, characterized in that: The method for extracting bamboo raw fibers is as follows: pretreated bamboo chips are added to an immobilized pectinase buffer solution and enzymatically hydrolyzed at 45–55°C for 2–3 hours. After filtration, the intermediate product is rinsed with deionized water and then added again to a mixed buffer solution of immobilized xylanase and immobilized laccase. After enzymatic hydrolysis at 45–55°C for 1–2 hours, the product is filtered, rinsed with deionized water, and dried at 40–50°C for 20–30 minutes to obtain bamboo raw fibers. The bamboo raw fibers are then fed into a carding machine for carding to obtain bamboo raw fibers for textile use.
7. The method for preparing bamboo fiber for textiles according to claim 6, characterized in that: In the method for extracting bamboo fiber, The mass ratio of pretreated bamboo strips to immobilized pectinase buffer was 0.9–1.1:28–32; The immobilized pectinase in the immobilized pectinase buffer contains 3-4% by mass. The mass ratio of the intermediate product, immobilized xylanase, and immobilized laccase in the mixed buffer was 0.9–1.1:28–32. In the mixed buffer of immobilized xylanase and immobilized laccase, the mass fraction of immobilized xylanase was 1.5–2.1%, and the mass fraction of immobilized laccase was 0.7–0.9%. Bamboo fiber for textiles has a fineness of 5.5–6.5 dtex.