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

By performing aminating modification and co-hydrolysis and co-condensation reaction on microcrystalline cellulose, a solid smooth layer is prepared in combination with AP binder, which solves the problems of easy contamination of cotton fabrics and lubricant depletion, and achieves durability and environmental protection of ultra-slip properties.

CN119145224BActive Publication Date: 2025-09-05JIANGSU NEW REBA TECH CO LTD +1
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Patent Information

Application Number
CN202411275235.1
Authority / Receiving Office
CN · China
Patent Type
Patents(China)
Current Assignee / Owner
Filing Date
2024-09-12
Publication Date
2025-09-05
Estimated Expiration
2044-09-12

AI Technical Summary

Technical Problem

Existing cotton fabrics are easily contaminated by common liquids, and existing superhydrophobic surface lubricants are easily depleted, affecting the surface smoothness.

Method used

The microcrystalline cellulose was amino-modified by 3-aminopropyltrimethoxysilane, and reacted with cetyltrimethoxysilane and (3-glycidyloxypropyl)trimethoxysilane, combined with Al(OH)3 and H3PO4 aqueous solution to prepare an AP binder, and organized onto the cotton fabric to form a solid smooth layer.

Benefits of technology

The prepared bio-based microcrystalline cellulose ultra-smooth cotton fabric has excellent physical durability and chemical stability, anti-fouling performance, and is green, environmentally friendly and low-cost.

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Abstract

The present invention discloses a method for preparing a bio-based microcrystalline cellulose super-smooth cotton fabric, comprising the following steps: (1) amminating microcrystalline cellulose with 3-aminopropyltrimethoxysilane; (2) adding the aminated microcrystalline cellulose to a reactive solution of hexadecyltrimethoxysilane and (3-glycidyloxypropyl)trimethoxysilane, and reacting in a water bath to obtain modified microcrystalline fiber; (3) mixing Al(OH)3 with an aqueous H3PO4 solution, heating and stirring the mixture to react, and preparing an AP binder; (4) mixing the modified microcrystalline cellulose with the AP binder, applying the mixture to a cotton fabric, and baking the mixture to obtain the bio-based microcrystalline cellulose super-smooth cotton fabric. The method of the present invention has a simple process, low cost, and is environmentally friendly. The super-smooth cotton fabric obtained has good anti-fouling properties, and the coating has excellent acid and alkali resistance and wear resistance.
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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 a comfortable lifestyle, the application of bio-based materials in the textile field has gradually increased. Cotton fabric, as a natural fiber fabric, has the advantages of being soft, breathable, renewable, and environmentally friendly, and is widely used in clothing, interior decoration, outdoor protection and other fields. However, in actual use, cotton fabric, which is mainly composed of cellulose, is easily stained by common liquids such as milk, coffee, cola, soy sauce, and vegetable oil. Therefore, the development of a new cotton fabric that combines the environmentally friendly properties of bio-based materials with ultra-slip properties has become a research hotspot in the textile industry.

[0003] Inspired by pitcher plants, researchers began experimenting with artificially constructed SLIPS surfaces and quickly discovered that these remarkable surfaces could be created by simply upgrading superhydrophobic surfaces. While water repellent, these microstructured superhydrophobic surfaces are highly receptive to certain fluorinated liquid organic compounds, allowing them to wet them. Therefore, if these liquids are applied to a superhydrophobic surface, they remain there for extended periods, resisting drainage. Water droplets on such surfaces, however, remain stuck to the surface, as they neither wet the superhydrophobic surface nor dissolve in the fluorinated liquid. However, the surface, slippery due to the fluorinated liquid layer, slides off with even the slightest tilt. However, over extended use, the impregnated lubricant in SLIPS is easily depleted, evaporates, and migrates, inevitably compromising the slipperiness of the embedded liquid. To overcome these limitations, "liquid-like" superslippery surfaces—solid slippery surfaces—have been introduced, devoid of any impregnated lubricant. 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 microcrystalline cellulose ultra-smooth cotton fabric. The method of the present invention is simple in process, low in cost, and 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 bio-based microcrystalline cellulose ultra-smooth cotton fabric, the preparation method comprising the following steps:

[0007] (1) Aminated microcrystalline cellulose was prepared by aminated microcrystalline cellulose using 3-aminopropyltrimethoxysilane (APTMS);

[0008] (2) adding the aminated microcrystalline cellulose to a reactive solution of hexadecyltrimethoxysilane (HDTMS) and (3-glycidyloxypropyl)trimethoxysilane (GPTMS) and reacting them in a water bath to obtain modified microcrystalline cellulose;

[0009] (3) Al(OH)3 and H3PO4 aqueous solution are mixed, heated and stirred to react, and an AP adhesive is prepared;

[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 washed with deionized water 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-glycidoxypropyl)trimethoxysilane (GPTMS) is 1:1-2.

[0015] In one embodiment of the present invention, in step (2), the mass volume ratio of the amino-modified microcrystalline cellulose to hexadecyltrimethoxysilane is 2-4:5 g / mL.

[0016] In one embodiment of the present invention, in step (2), the water bath reaction conditions 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 prepare a reactive solution; the amino-modified microcrystalline cellulose prepared in step (1) is added to the above-mentioned reactive solution and stirred in a water bath at 100° C. for reaction for 3 hours. After the reaction is completed, the microcrystalline cellulose powder is fully washed with deionized water 3-5 times to remove unreacted reagents, and the powder is dried in an oven at 80° C. to prepare modified microcrystalline fiber.

[0018] In one embodiment of the present invention, in step (3), the molar ratio of Al(OH)3 to H3PO4 is 1:3.

[0019] In one embodiment of the present invention, in step (3), the concentration of the H3PO4 aqueous solution is 65%.

[0020] In one embodiment of the present invention, in step (3), the heating and stirring reaction conditions are: 90-100° C. for 3 h.

[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 minutes.

[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 onto cotton fabric, and baked in a drying machine at 120-150° C. for 1-3 minutes 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 easily available, no expensive reagents are required, and the reaction conditions are mild. The co-hydrolysis and co-condensation of the organic silane mixture and the epoxyamine ring-opening reaction at the interface of the present invention produce a highly strong, transparent, "liquid" solid smooth omniphobic coating.

[0026] The present invention uses bio-based microcrystalline cellulose as a base, is green, non-toxic, and eco-friendly, and the modified microcrystalline cellulose is tightly bonded to the 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, as well as excellent anti-fouling properties. DETAILED DESCRIPTION

[0027] The present invention will be described in detail below with reference to the embodiments.

[0028] Sliding angle test method: The sliding angle tester is a special instrument for measuring 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] Example 1:

[0030] A method for preparing a bio-based microcrystalline cellulose ultra-smooth cotton fabric comprises the following steps:

[0031] (1) 5 g of microcrystalline cellulose powder was added to 15 g of 3-aminopropyltrimethoxysilane (APTMS) solution and reacted in a 60°C water bath for 30 min to fully aminize the surface of the microcrystalline cellulose powder. The microcrystalline cellulose powder was washed with deionized water 3-5 times to remove unreacted 3-aminopropyltrimethoxysilane (APTMS), and the powder was dried in an oven at 80°C to obtain aminated microcrystalline cellulose.

[0032] (2) 5 mL of hexadecyltrimethoxysilane (HDTMS) and 10 mL of (3-glycidyloxypropyl)trimethoxysilane (GPTMS) were added to 20 mL of ethanol solution and stirred for reaction for 30 minutes to prepare a reactive solution; 2.22 g of amino-modified microcrystalline cellulose powder was added to the reactive solution and stirred in a water bath at 100°C for 3 hours, the microcrystalline cellulose powder was thoroughly washed with deionized water 3-5 times to remove unreacted reagents, and the powder was dried in an oven at 80°C to prepare modified microcrystalline cellulose;

[0033] (3) 5 g of Al(OH)3 was mixed with 18.85 g of phosphoric acid (H3PO4) and stirred at 100°C for 3 h to prepare an AP adhesive. Before preparation, 85% phosphoric acid (H3PO4) was diluted to 65% by adding deionized water.

[0034] (4) 2 g of modified microcrystalline cellulose powder was thoroughly mixed with 4 g of AP binder and printed onto cotton fabric. The fabric was then baked in a drying oven at 150°C for 3 min to obtain a bio-based ultra-smooth cotton fabric with a sliding angle of 15.6°.

[0035] Example 2:

[0036] Same as Example 1, except that the amount of (3-glycidyloxypropyl)trimethoxysilane (GPTMS) added in step (2) was 5 mL. The sliding angle was 17.9°.

[0037] Example 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] Example 4:

[0040] Same as Example 1, except that the baking temperature in step (4) is 120°C and the baking time is 1 minute. The sliding angle is 20.8°.

[0041] 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 microcrystalline cellulose ultra-smooth cotton fabric, characterized in that: The preparation method comprises the following steps: (1) Aminated microcrystalline cellulose was modified by 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 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 an 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 amination 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 carried out by printing; the baking conditions are: baking at 120-150° C. for 1-3 minutes.

Citation Information

Patent Citations

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