Preparation method of bio-based microcrystalline cellulose super-smooth cotton fabric
By aminating modification of microcrystalline cellulose and silane reaction, combined with the use of AP binder, the problems of bio-based cotton fabric contamination and lubricant depletion were solved, and biological with excellent durability and anti-fouling properties were prepared. Base microcrystalline cellulose ultra-sliding cotton fabric.
Patent Information
- Application Number
- CN202411275235.1
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2024-09-12
- Publication Date
- 2024-12-17
- Estimated Expiration
- 2044-09-12
AI Technical Summary
Existing bio-based cotton fabrics are prone to contamination when exposed to common liquids, and the superhydrophobic surface is easily depleted during long-term use, affecting the smoothness of the surface.
The microcrystalline cellulose is amino-modified by 3-aminopropyltrimethoxysilane and reacted with cetyltrimethoxysilane and glycidyloxypropyltrimethoxysilane to form modified microcrystalline Cellulose, combined with Al(OH)3 and H3PO4 aqueous solution, AP binder was prepared, and it was organized on cotton fabrics by printing to bake them to prepare solid and smooth bio-based microcrystalline cellulose ultra-sliding cotton fabric.
Achieves low-cost preparation without expensive reagents, resulting in a highly robust, transparent solid smooth fully sparse coating, enhancing the wash resistance and stain resistance of cotton fabrics, with excellent physical durability and chemical stability.
Abstract
Description
Technical Field
[0001] The invention relates to the technical field of textile processing, in particular to a method for preparing a bio-based microcrystalline cellulose ultra-smooth cotton fabric. Background Art
[0002] In recent years, with the rapid development of the textile industry and people's pursuit of environmental protection and comfortable life, the application of bio-based materials in the textile field has gradually increased. As one of the natural fiber fabrics, cotton fabric has the advantages of softness, breathability, renewability, and environmental protection. It is widely used in clothing, interior decoration, outdoor protection and other fields. However, in actual use, cotton fabrics with cellulose as the main component are easily stained by common liquids such as milk, coffee, cola, soy sauce, and vegetable oil. Therefore, the development of a new type of cotton fabric that has both the environmental protection characteristics of bio-based materials and super-slip properties has become a research hotspot in the textile industry.
[0003] Inspired by the pitcher plant, researchers began to try to artificially construct SLIPS surfaces, and soon discovered that this extraordinary surface can be simply "upgraded" from a superhydrophobic surface. Although the superhydrophobic surface covered with microstructures does not get wet, it is "like-minded" with some fluorine-containing liquid organics and can be wetted by the latter. Therefore, if these liquids are applied to the superhydrophobic surface, they can stay there for a long time without flowing away. If we drop water on such a surface, since water can neither wet the superhydrophobic surface nor dissolve in these fluorine-containing liquids, it can only stay on the surface, and the surface is very smooth due to the presence of the fluorine-containing liquid layer, so as long as we tilt it slightly, the water drop will slide down. However, during long-term use, the injected lubricant in SLIPS is easily exhausted, volatilized and migrated, which inevitably damages the smoothness of the surface embedded liquid. In order to overcome these limitations, a "liquid-like" supersmooth surface without any injected lubricant, that is, a solid smooth surface, was introduced. Summary of the invention
[0004] In view of the above problems existing in the prior art, the present invention provides a method for preparing bio-based microcrystalline 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 microcrystalline cellulose ultra-smooth cotton fabric, the preparation method comprising the following steps:
[0007] (1) Aminated microcrystalline cellulose is modified by 3-aminopropyltrimethoxysilane (APTMS) to obtain aminated microcrystalline cellulose;
[0008] (2) adding the aminated microcrystalline cellulose to a reactive solution of hexadecyltrimethoxysilane (HDTMS) and (3-glycidyloxypropyl)trimethoxysilane (GPTMS), and reacting in a water bath to obtain modified microcrystalline cellulose;
[0009] (3) Al(OH) 3 With H 3 PO 4 The aqueous solutions are mixed, heated and stirred for reaction to prepare an AP adhesive;
[0010] (4) The modified microcrystalline cellulose prepared in step (2) is mixed with the AP adhesive prepared in step (3), and the mixture is applied to cotton fabric and baked to obtain the bio-based microcrystalline cellulose ultra-smooth cotton fabric.
[0011] In one embodiment of the present invention, in step (1), the conditions for the amino modification are: reaction at 60-80° C. for 30 min.
[0012] In one embodiment of the present invention, in step (1), the mass ratio of 3-aminopropyltrimethoxysilane to microcrystalline cellulose is 3:1.
[0013] In one embodiment of the present invention, in step (1), microcrystalline cellulose powder is added to a 3-aminopropyltrimethoxysilane (APTMS) solution and reacted in a water bath at 60-80°C for 30 minutes to fully aminize the surface of the microcrystalline cellulose powder, the microcrystalline cellulose powder is fully washed with deionized water for 3-5 times to remove unreacted 3-aminopropyltrimethoxysilane (APTMS), and the powder is dried in an oven at 80°C to obtain aminated microcrystalline cellulose.
[0014] In one embodiment of the present invention, in step (2), the volume ratio of hexadecyltrimethoxysilane (HDTMS) to (3-glycidyloxypropyl)trimethoxysilane (GPTMS) is 1:1-2.
[0015] In one embodiment of the present invention, in step (2), the mass volume ratio of the aminated microcrystalline cellulose to hexadecyltrimethoxysilane is 2-4:5 g / mL.
[0016] In one embodiment of the present invention, in step (2), the conditions for the water bath reaction are: 90-100° C. for 3 h.
[0017] In one embodiment of the present invention, in step (2), 5 mL of hexadecyltrimethoxysilane (HDTMS) and 5-10 mL of (3-glycidyloxypropyl)trimethoxysilane (GPTMS) are added to 20 mL of ethanol solution and stirred for reaction for 15-30 minutes to obtain a reactive solution; the amino-modified microcrystalline cellulose obtained in step (1) is added to the above-mentioned reactive solution and stirred for reaction in a water bath at 100° C. for 3 hours. After the reaction is completed, the microcrystalline cellulose powder is fully washed with deionized water for 3-5 times to remove unreacted reagents, and the powder is dried in an oven at 80° C. to obtain modified microcrystalline fibers.
[0018] In one embodiment of the present invention, in step (3), Al(OH) 3 With H 3 PO 4 The molar ratio is 1:3.
[0019] In one embodiment of the present invention, in step (3), H 3 PO 4 The concentration of the aqueous solution was 65%.
[0020] In one embodiment of the present invention, in step (3), the heating and stirring reaction conditions are: reacting at 90-100° C. for 3 hours.
[0021] In one embodiment of the present invention, in step (4), the mass ratio of the modified microcrystalline cellulose to the AP binder is 1:2.
[0022] In one embodiment of the present invention, in step (4), the finishing is performed by printing; and the baking conditions are: baking at 120-150° C. for 1-3 min.
[0023] In one embodiment of the present invention, in step (4), the modified microcrystalline cellulose prepared in step (2) is mixed with the AP adhesive prepared in step (3), printed on cotton fabric, and baked in a drying machine at 120-150° C. for 1-3 min to obtain a bio-based ultra-smooth cotton fabric.
[0024] The beneficial technical effects of the present invention are:
[0025] The raw materials of the present invention are cheap and easy to obtain, no expensive reagents are needed, and the reaction conditions are mild; the co-hydrolysis and co-condensation of the organic silane mixture used in the present invention and the epoxyamine ring-opening reaction at the interface produce a highly strong, transparent, "liquid" solid smooth fully hydrophobic coating.
[0026] The present invention uses bio-based microcrystalline cellulose as a base, is green and non-toxic, and is friendly to the ecological environment. The modified microcrystalline cellulose is tightly combined with cotton fabric through an AP adhesive, thereby enhancing the washability of the ultra-smooth cotton fabric. The prepared ultra-smooth cotton fabric has excellent physical durability and chemical stability, and has excellent anti-fouling performance. DETAILED DESCRIPTION
[0027] The present invention will be described in detail below in conjunction with the embodiments.
[0028] Sliding angle test method: The sliding angle tester is a special instrument for measuring the friction angle. The design standard follows DIN53119-2-1997. It adopts advanced single-screw guide column mechanical structure, motor control and angle digital display, and has high control accuracy. The equipment is used to test the anti-slip performance of the super-slip fabric of this embodiment, and its friction performance is evaluated by testing the sliding angle between the fabric and the plane. During the test, the fabric is driven by an electric drive 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. 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.
[0029] Embodiment 1:
[0030] A method for preparing a bio-based microcrystalline cellulose ultra-smooth cotton fabric comprises the following steps:
[0031] (1) adding 5 g of microcrystalline cellulose powder to 15 g of 3-aminopropyltrimethoxysilane (APTMS) solution, and reacting in a water bath at 60° C. for 30 min to fully aminize the surface of the microcrystalline cellulose powder, washing the microcrystalline cellulose powder with deionized water for 3-5 times to remove unreacted 3-aminopropyltrimethoxysilane (APTMS), and drying the powder in an oven at 80° C. to obtain aminated microcrystalline cellulose;
[0032] (2) adding 5 mL of hexadecyltrimethoxysilane (HDTMS) and 10 mL of (3-glycidyloxypropyl)trimethoxysilane (GPTMS) to 20 mL of ethanol solution and stirring for reaction for 30 min to prepare a reactive solution; adding 2.22 g of amino-modified microcrystalline cellulose powder to the reactive solution and stirring for reaction in a water bath at 100° C. for 3 h, washing the microcrystalline cellulose powder with deionized water for 3-5 times to remove unreacted reagents, and drying the powder in an oven at 80° C. to prepare modified microcrystalline cellulose;
[0033] (3) 5g Al(OH) 3With 18.85g phosphoric acid (H 3 PO 4 ) were mixed and stirred at 100°C for 3 h to prepare the AP adhesive. Before preparation, 85% phosphoric acid (H 3 PO 4 ) was diluted to 65% by adding deionized water.
[0034] (4) 2 g of the modified microcrystalline cellulose powder was fully mixed with 4 g of AP binder, and printed on cotton fabric, which was then baked in a baking machine at 150° C. for 3 min to obtain a bio-based ultra-smooth cotton fabric with a sliding angle of 15.6°.
[0035] Embodiment 2:
[0036] Same as Example 1, except that the amount of (3-glycidyloxypropyl)trimethoxysilane (GPTMS) added in step (2) is 5 mL. The sliding angle is 17.9°.
[0037] Embodiment 3:
[0038] Same as Example 1, except that the reaction time of HDTMS and GPTMS in step (2) is 15 min. The sliding angle is 18.2°.
[0039] Embodiment 4:
[0040] Same as Example 1, except that the baking temperature in step (4) is 120°C and the baking time is 1 min. The sliding angle is 20.8°.
[0041] 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 microcrystalline cellulose ultra-smooth cotton fabric, characterized in that: The preparation method comprises the following steps: (1) Amination modification of microcrystalline cellulose is performed using 3-aminopropyltrimethoxysilane to obtain aminated microcrystalline cellulose; (2) adding the aminated microcrystalline cellulose to a reactive solution of hexadecyltrimethoxysilane and (3-glycidyloxypropyl)trimethoxysilane, and reacting them in a water bath to obtain modified microcrystalline cellulose; (3) Al(OH)3 and H3PO4 aqueous solution are mixed, heated and stirred to react, and AP adhesive is prepared; (4) The modified microcrystalline cellulose prepared in step (2) is mixed with the AP adhesive prepared in step (3), and the mixture is applied to cotton fabric and baked to obtain the bio-based microcrystalline cellulose ultra-smooth cotton fabric.
2. The preparation method according to claim 1, characterized in that: In step (1), the conditions for the amino modification are: reaction at 60-80°C for 30 minutes.
3. The preparation method according to claim 1, characterized in that: In step (1), the mass ratio of 3-aminopropyltrimethoxysilane to microcrystalline cellulose is 3:
1.
4. The preparation method according to claim 1, characterized in that: In step (2), the volume ratio of hexadecyltrimethoxysilane to (3-glycidyloxypropyl)trimethoxysilane is 1:1-2.
5. The preparation method according to claim 1, characterized in that: In step (2), the mass volume ratio of the amino-modified microcrystalline cellulose to hexadecyltrimethoxysilane is 2-4:5 g / mL.
6. The preparation method according to claim 1, characterized in that: In step (2), the conditions for the water bath reaction are: 90-100° C. for 3 h.
7. The preparation method according to claim 1, characterized in that: In step (3), the molar ratio of Al(OH)3 to H3PO4 is 1:
3.
8. The preparation method according to claim 1, characterized in that: In step (3), the heating and stirring reaction conditions are: 90-100° C. for 3 h.
9. The preparation method according to claim 1, characterized in that: In step (4), the mass ratio of modified microcrystalline cellulose to AP binder is 1:
2.
10. The preparation method according to claim 1, characterized in that: In step (4), the finishing is performed by printing; the baking conditions are: baking at 120-150° C. for 1-3 minutes.
Citation Information
Patent Citations
Method for preparing durable cellulose fiber fabric with super-hydrophobic surface
CN104594028A
All-water-based super-hydrophobic coating with reversible wettability as well as preparation method and application thereof
CN113774655A
Inorganic binder reinforced fluoride-free self-repairing super-hydrophobic spray and preparation and use methods thereof
CN113881253A
Method for preparing nano cellulose by using papermaking refined pulp as raw material
CN116411474A
Polyurethane of increased of biomass-content as well as improvement of material property by filling or reacting modified-microcrystalline cellulose , and preparation methods thereof
KR1020180128364A
