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

Abstract

The invention discloses a preparation method of a bio-based nano-crystal cellulose super-smooth cotton fabric. The preparation method comprises the following steps: (1) modifying nano-crystal cellulose by adopting 3-mercaptopropyltriethoxysilane; (2) acetone and vinyl trimethoxy silane are mixed, concentrated hydrochloric acid and deionized water are dropwise added, stirring reflux is performed, and octavinyl octasilsesquioxane is prepared; (3) adding the modified nanocrystalline cellulose into a mixed solution containing dichloromethane, octavinyl octasilsesquioxane, pentaerythritol tetra-3-mercaptopropionate, vinyl-terminated polydimethylsiloxane and benzoin dimethyl ether, sealing the mixed solution, and irradiating the mixed solution with ultraviolet light; and (4) carrying out padding treatment on the cotton fabric by adopting the product in the step (3), and then carrying out pre-drying and high-temperature baking to obtain the bio-based nano-crystal cellulose super-smooth cotton fabric. The method disclosed by the invention is simple in process, relatively low in cost and environment-friendly, and the obtained super-smooth cotton fabric has excellent antifouling property, acid and alkali resistance, wear resistance and the like.

Description

Technical Field

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

[0002] Textiles are widely used in household products, industrial manufacturing, medical and health care, agriculture and forestry due to their high flexibility, high specific surface area and diverse material sources. However, textiles will inevitably come into contact with various substances during use, such as food, oily liquids, cosmetics, etc. These substances are easy to adhere to the surface of the fabric, thereby reducing its aesthetics, comfort and service life. Therefore, the development of fabrics with high-efficiency antifouling properties has become a hot topic in the field of textiles today.

[0003] The rough structure of the rim of the pitcher plant 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-nano porous substrates. The "super-slippery" in its name refers to the low surface energy, low liquid adhesion and extremely low friction coefficient of such surfaces. The introduction of the concept of super-slippery surface can provide new ideas for the construction of anti-fouling textiles. However, unlike the traditional super-slippery surface construction substrate, 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 view of the above problems existing in the prior art, the present invention provides a method for preparing a 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 solution of the present invention is 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 is modified by using 3-mercaptopropyltriethoxysilane (MPTES) to obtain modified nanocrystalline cellulose;

[0008] (2) Acetone and vinyl trimethoxysilane (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 octavinyl octasilsesquioxane (OV-POSS);

[0009] (3) adding the modified nanocrystalline cellulose prepared in step (1) into 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 for 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 obtain 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; 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 octavinyl octasilsesquioxane (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 dimethyl benzoate (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 light irradiation are: an intensity of 300 W / m 2 Irradiate with 360nm UV light for 1h.

[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 min; and the baking conditions are: baking at 150°C for 1-5 min.

[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 used to synthesize POSS, and a thiol-ene click reaction is further used to prepare a POSS functionalized polymer, and the preparation method is simple and efficient.

[0022] The present 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 in conjunction with the embodiments.

[0025] Sliding angle test method: The sliding angle tester is a special instrument used to measure the friction angle. The design standard follows DIN53119-2-1997. It adopts the advanced mechanical structure of single screw guide column, motor control and angle digital display, and has high control accuracy. This equipment is used to test the anti-slip performance of fabrics and evaluate their friction performance by testing the sliding angle between the fabric and the plane. During the test, the fabric is driven by electricity to slide on the platform at a certain speed, and the angle at which the fabric starts to slide is recorded by the LCD digital display, which is its sliding angle.

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

[0027] Embodiment 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 in a volume ratio of 5:1, and stirred in a water bath at 80° C. for 30 min, so that the -OH on the surface of the nanocrystalline cellulose can be fully replaced by -SH, thereby obtaining modified nanocrystalline cellulose;

[0030] (2) 1350 mL of acetone and 133.5 g of vinyltrimethoxysilane (VTMS) were charged into a 2 L flask equipped with a magnetic stirrer, and then 225 mL of concentrated hydrochloric acid (38 wt%) and 259.2 mL of deionized water were added. The mixture was stirred and refluxed 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 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 Irradiate with 360nm UV light for 1h.

[0032] (4) The cotton fabric was treated with the solution obtained in step (3) by dipping and padding, and the sample was washed with anhydrous ethanol for 3 times to remove the residual reactants. The treated cotton fabric was pre-baked in an oven at 60° C. for 30 min, and finally baked in a baking machine at 150° C. for 3 min to obtain a bio-based ultra-smooth cotton fabric. The sliding angle was tested to be 12.8°.

[0033] Embodiment 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] Embodiment 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] Embodiment 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, and the steps described are not intended to limit the execution order thereof. Those skilled in the art may make obvious improvements to the present invention in combination with existing common knowledge, which also fall within the scope of protection defined by the claims of the present invention.

Claims

1. A method for preparing a bio-based nanocrystalline cellulose ultra-smooth cotton fabric, characterized in that: The preparation method comprises the following steps: (1) using 3-mercaptopropyltriethoxysilane to modify nanocrystalline cellulose to obtain modified nanocrystalline cellulose; (2) Acetone and vinyltrimethoxysilane are mixed, concentrated hydrochloric acid and deionized water are added dropwise, and the mixture is stirred and refluxed. During the reaction, a white solid is deposited, which is centrifuged, washed with ethanol, vacuum dried, and recrystallized to obtain octavinyloctasilsesquioxane; (3) adding the modified nanocrystalline cellulose obtained 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 for 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 obtain 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 38wt%; 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 uses 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 octavinyl octasilsesquioxane 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 conditions for ultraviolet irradiation are: intensity of 300W / m 2 Irradiate with 360nm UV light for 1h.

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 min; and the baking conditions are: baking at 150° C. for 1-5 min.