Preparation method of bio-based nanocrystalline cellulose ultra-smooth cotton fabric

Abstract

The invention discloses a method for preparing a bio-based nanocrystalline cellulose super-smooth cotton fabric, comprising the following steps: (1) modifying nanocrystalline cellulose using 3-mercaptopropyltriethoxysilane; (2) mixing acetone and vinyltrimethoxysilane, then dropping concentrated hydrochloric acid and deionized water, stirring and refluxing to obtain octavinyloctasilsesquioxane; (3) adding modified nanocrystalline cellulose to a mixed solution containing dichloromethane, octavinyloctasilsesquioxane, pentaerythritol tetra-3-mercaptopropionate, terminal vinyl polydimethylsiloxane and benzoin dimethyl ether, sealing, and irradiating with ultraviolet light; (4) padding the cotton fabric with the product of step (3), followed by pre-baking and high-temperature baking to obtain bio-based nanocrystalline cellulose super-smooth cotton fabric. The method of the present invention is simple in process, low in cost, environmentally friendly, and the obtained super-smooth cotton fabric has good anti-fouling performance, excellent acid and alkali resistance, and wear resistance.

Description

Technical Field

[0001] The present invention relates to the technical field of textile processing, in particular to a method for preparing a bio-based nanocrystalline cellulose ultra-smooth cotton fabric. Background Art

[0002] Textiles, due to their high flexibility, high surface area, and diverse material sources, are widely used in household products, industrial manufacturing, healthcare, agriculture, and forestry. However, during use, textiles inevitably come into contact with various substances, such as food, oils, and cosmetics. These substances easily adhere to the fabric surface, reducing its aesthetics, comfort, and service life. Therefore, the development of fabrics with effective antifouling properties has become a hot topic in the textile field.

[0003] The rough structure of the rim of the pitcher plant mouth can form an ultra-smooth liquid surface with low adhesion by storing substances such as mucus. Inspired by this mechanism, researchers proposed the concept of liquid-infused super-slippery surface (SLIPS). This surface is an emerging anti-fouling material prepared by injecting liquid lubricants into micro-nanoporous substrates. The "super-slippery" in its name refers to the fact that this type of surface has low surface energy, low liquid adhesion and extremely low friction coefficient. The introduction of the concept of super-slippery surface can provide new ideas for the construction of anti-fouling textiles. However, unlike traditional super-slippery surface construction substrates, the construction of super-slippery fabric surfaces is more complicated due to the presence of a large number of capillaries in the textiles themselves. Moreover, there is currently a lack of research on the mechanism of construction of super-slippery coatings on fabric surfaces and the application of their anti-fouling effects. Therefore, how to organically combine super-slippery anti-fouling coatings with textiles and improve the anti-fouling and performance stability of fabrics has important research significance and practical value. Summary of the Invention

[0004] In order to solve the above problems in the prior art, the present invention provides a method for preparing bio-based nanocrystalline cellulose ultra-smooth cotton fabric. The method of the present invention has simple process, low cost and is environmentally friendly.

[0005] The technical solutions of the present invention are as follows:

[0006] The first object of the present invention is to provide a method for preparing a bio-based nanocrystalline cellulose ultra-smooth cotton fabric, the preparation method comprising the following steps:

[0007] (1) Nanocrystalline cellulose was modified with 3-mercaptopropyltriethoxysilane (MPTES) to obtain modified nanocrystalline cellulose;

[0008] (2) Acetone and vinyltrimethoxysilane (VTMS) were mixed, concentrated hydrochloric acid and deionized water were added dropwise, and the mixture was stirred and refluxed. During the reaction, a white solid was deposited, which was centrifuged, washed with ethanol, vacuum-dried, and recrystallized to obtain octavinyloctasilsesquioxane (OV-POSS);

[0009] (3) adding the modified nanocrystalline cellulose prepared in step (1) to a mixed solution containing dichloromethane, octavinyl octasilsesquioxane (OV-POSS), pentaerythritol tetrakis-3-mercaptopropionate (PETMP), vinyl-terminated polydimethylsiloxane (ViPDMS) and dimethyl benzoate (DMPA), sealing the solution and irradiating the solution with ultraviolet light;

[0010] (4) The product obtained in step (3) is used to perform padding treatment on cotton fabric, and the sample is washed with anhydrous ethanol multiple times to remove residual reactants, and then pre-baked and high-temperature baked to obtain the bio-based nanocrystalline cellulose ultra-smooth cotton fabric.

[0011] In one embodiment of the present invention, in step (1), 3-mercaptopropyltriethoxysilane (MPTES) and nanocrystalline cellulose emulsion are mixed in a volume ratio of 5:1 and stirred in a water bath at 80° C. for 30 minutes to prepare modified nanocrystalline cellulose.

[0012] In one embodiment of the present invention, the solid content of the nanocrystalline cellulose emulsion is 10-15%.

[0013] In one embodiment of the present invention, in step (2), the volume mass ratio of acetone to vinyltrimethoxysilane (VTMS) is 10-15:1 mL / g.

[0014] In one embodiment of the present invention, in step (2), the concentration of concentrated hydrochloric acid is 38%; and the volume ratio of concentrated hydrochloric acid to deionized water is 1:1.1-1.2.

[0015] In one embodiment of the present invention, in step (2), the stirring and reflux conditions are: stirring and reflux at 40°C for 48 hours; the vacuum drying temperature is 60°C; the recrystallization uses a mixed solvent of dichloromethane and acetone; and the volume ratio of dichloromethane to acetone is 1:3.

[0016] In one embodiment of the present invention, in step (3), the solvent in the mixed solution is dichloromethane, the mass fraction of octavinyloctasilsesquioxane (OV-POSS) is 0.5-3%, the amount of pentaerythritol tetrakis-3-mercaptopropionate (PETMP) is 0.5-2%, the amount of vinyl-terminated polydimethylsiloxane (ViPDMS) is 0.5-3%, and the amount of benzoin dimethyl ether (DMPA) is 0.02-0.2%.

[0017] In one embodiment of the present invention, in step (3), the mass ratio of modified nanocrystalline cellulose to the mixed solution is 1:30-40.

[0018] In one embodiment of the present invention, in step (3), the conditions for ultraviolet irradiation are: an intensity of 300W / m 2 The samples were irradiated with 360 nm ultraviolet light for 1 h.

[0019] In one embodiment of the present invention, in step (3), the padding treatment is a one-dip and one-pad treatment; the pre-baking conditions are: pre-baking at 60°C for 10-30 minutes; and the baking conditions are: baking at 150°C for 1-5 minutes.

[0020] The beneficial technical effects of the present invention are:

[0021] The raw materials required by the invention are cheap and easily available, no expensive catalyst is needed, and the reaction conditions are mild; a simple hydrolysis condensation reaction is adopted to synthesize POSS, and a thiol-ene click reaction is further adopted to prepare a POSS functionalized polymer; and the preparation method is simple and efficient.

[0022] The invention adds vinyl polydimethylsiloxane (ViPDMS) to the POSS polymer, reduces the surface energy of the coating, effectively enhances the antifouling performance of the cotton fabric surface, and the prepared super-smooth cotton fabric has good acid and alkali resistance and friction resistance and other properties.

[0023] The invention uses biomass as the substrate, is environmentally friendly, has a simple production method, mild reaction conditions during the production process, is easy to operate, and has low cost. DETAILED DESCRIPTION

[0024] The present invention will be described in detail below with reference to the embodiments.

[0025] Sliding Angle Test Method: The sliding angle tester is a specialized instrument for measuring friction angles. Designed in accordance with DIN 53119-2-1997, it utilizes an advanced single-screw guide mechanism, motor control, and a digital angle display, resulting in high control precision. This device is used to test the anti-slip properties of fabrics by measuring the sliding angle between the fabric and a flat surface to assess friction performance. During the test, the fabric is electrically driven to slide at a constant speed across a platform. The LCD digital display records the angle at which the fabric begins to slide, representing the sliding angle.

[0026] The main technical parameters of the sliding angle tester include a test angle range of 0-40°, a test speed of 2° / second, a platform area of ​​600×500mm, a maximum load of 50KG, a machine weight of approximately 80KG, and a volume of 750×550×550mm.

[0027] Example 1:

[0028] A method for preparing a bio-based nanocrystalline cellulose ultra-smooth cotton fabric comprises the following steps:

[0029] (1) 3-Mercaptopropyltriethoxysilane (MPTES) and a nanocrystalline cellulose emulsion with a solid content of 15% were added to a beaker at a volume ratio of 5:1 and stirred in a water bath at 80°C for 30 min to allow the -OH groups on the surface of the nanocrystalline cellulose to be fully replaced by -SH groups to obtain modified nanocrystalline cellulose;

[0030] (2) 1350 mL of acetone and 133.5 g of vinyltrimethoxysilane (VTMS) were placed in a 2 L flask equipped with a magnetic stirrer. 225 mL of concentrated hydrochloric acid (38 wt%) and 259.2 mL of deionized water were added and stirred at 40 ° C for 48 h. White solids were deposited on the wall of the flask and the reaction solution was brown. The solvent mixture was poured into a pre-prepared 2 L beaker for reuse in the next experiment. The white solid precipitate was centrifuged, washed with ethanol, and dried in a vacuum drying oven at 60 ° C to obtain a crude product. The total crude product was then recrystallized with a mixed solvent of dichloromethane and acetone (volume ratio of 1:3) to obtain octavinyl octasilsesquioxane (OV-POSS).

[0031] (3) 10 g of modified nanocrystalline cellulose was added to a 500 mL beaker containing a mixed solution of 225 mL of dichloromethane, 4.0 g of octavinyl octasilsesquioxane (OV-POSS), 4.0 g of pentaerythritol tetrakis-3-mercaptopropionate (PETMP), 3.0 g of vinyl-terminated polydimethylsiloxane (ViPDMS), and 0.20 g of dimethyl benzoate (DMPA); the beaker was then sealed and heated with a pressure of 300 W / m 2 The samples were irradiated with 360 nm ultraviolet light for 1 h.

[0032] (4) The solution obtained in step (3) was used to perform a dip-pad treatment on a cotton fabric. The sample was washed three times with anhydrous ethanol to remove residual reactants. The treated cotton fabric was pre-dried in a 60°C oven for 30 minutes and finally dried in a drying oven at 150°C for 3 minutes to obtain a bio-based ultra-smooth cotton fabric. The sliding angle was measured to be 12.8°.

[0033] Example 2:

[0034] Referring to Example 1, the difference from Example 1 is that in step (3), the amount of pentaerythritol tetrakis-3-mercaptopropionate (PETMP) used is 2.0 g. The sliding angle is 16.9°.

[0035] Example 3:

[0036] Referring to Example 1, the difference from Example 1 is that in step (3), the amount of vinyl-terminated polydimethylsiloxane (ViPDMS) used is 2.0 g, and its sliding angle is 17.1°.

[0037] Example 4:

[0038] Referring to Example 1, the difference from Example 1 is that in step (3), the baking time is 1 min and the sliding angle is 18.2°.

[0039] The embodiments provided above are not intended to limit the scope of the present invention, nor are the steps described to limit their execution order. Any obvious improvements to the present invention made by those skilled in the art in combination with existing common knowledge shall fall within the scope of protection defined by the claims of the present invention.

Claims

1. A method for preparing bio-based nanocrystalline cellulose ultra-smooth cotton fabric, characterized in that: The preparation method comprises the following steps: (1) Nanocrystalline cellulose was modified with 3-mercaptopropyltriethoxysilane to obtain modified nanocrystalline cellulose; (2) Acetone and vinyltrimethoxysilane were mixed, concentrated hydrochloric acid and deionized water were added dropwise, and the mixture was stirred and refluxed. During the reaction, a white solid was deposited, which was centrifuged, washed with ethanol, vacuum dried, and recrystallized to obtain octavinyloctasilsesquioxane; (3) adding the modified nanocrystalline cellulose prepared in step (1) to a mixed solution containing dichloromethane, octavinyl octasilsesquioxane, pentaerythritol tetrakis-3-mercaptopropionate, vinyl-terminated polydimethylsiloxane, and benzoin dimethyl ether, sealing the solution, and irradiating the solution with ultraviolet light; (4) The product obtained in step (3) is used to perform padding treatment on cotton fabric, and the sample is washed with anhydrous ethanol multiple times to remove residual reactants, and then pre-baked and high-temperature baked to obtain the bio-based nanocrystalline cellulose ultra-smooth cotton fabric.

2. The preparation method according to claim 1, characterized in that In step (1), 3-mercaptopropyltriethoxysilane and nanocrystalline cellulose emulsion are mixed in a volume ratio of 5:1, and stirred in a water bath at 80° C. for 30 minutes to prepare modified nanocrystalline cellulose.

3. The preparation method according to claim 2, characterized in that The solid content of the nanocrystalline cellulose emulsion is 10-15%.

4. The preparation method according to claim 1, characterized in that In step (2), the volume mass ratio of acetone to vinyltrimethoxysilane is 10-15:1 mL / g.

5. The preparation method according to claim 1, characterized in that In step (2), the concentration of concentrated hydrochloric acid is 38 wt %; the volume ratio of concentrated hydrochloric acid to deionized water is 1:1.1-1.

2.

6. The preparation method according to claim 1, characterized in that In step (2), the stirring and reflux conditions are: stirring and reflux at 40° C. for 48 h; the vacuum drying temperature is 60° C.; and the recrystallization is carried out using a mixed solvent of dichloromethane and acetone; The volume ratio of dichloromethane to acetone is 1:

3.

7. The preparation method according to claim 1, characterized in that In step (3), the solvent in the mixed solution is dichloromethane, the mass fraction of octavinyloctasilsesquioxane is 0.5-3%, the mass fraction of pentaerythritol tetrakis-3-mercaptopropionate is 0.5-2%, the mass fraction of vinyl-terminated polydimethylsiloxane is 0.5-3%, and the mass fraction of benzoin dimethyl ether is 0.02-0.2%.

8. The preparation method according to claim 1, characterized in that In step (3), the mass ratio of modified nanocrystalline cellulose to the mixed solution is 1:30-40.

9. The preparation method according to claim 1, characterized in that In step (3), the UV irradiation conditions are: intensity of 300W / m 2 The samples were irradiated with 360 nm ultraviolet light for 1 h.

10. The preparation method according to claim 1, characterized in that In step (3), the padding treatment is a one-dip and one-pad treatment; the pre-baking conditions are: pre-baking at 60° C. for 10-30 minutes; and the baking conditions are: baking at 150° C. for 1-5 minutes.