Matting-modified cellulose fiber and method for manufacturing the same

EP4617412A3Pending Publication Date: 2025-10-22ACEGREEN ECO-MATERIAL TECHNOLOGY CO LTD
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Patent Information

Application Number
EP2025163190
Authority / Receiving Office
EP · EP
Patent Type
Applications
Current Assignee / Owner
Priority Date
2024-03-12
Filing Date
2025-03-12
Publication Date
2025-10-22

AI Technical Summary

Technical Problem

Conventional matting agents for cellulose fibers lack effective chemical bonding with the fiber surface, leading to poor adhesion and high residual content in spinning solvents, which increases processing costs and reduces recyclability.

Method used

A modified titanium dioxide matting agent with functional groups is used to form chemical bonds with cellulose fibers, enhancing adhesion and allowing for nearly complete recovery of the spinning solvent.

Benefits of technology

The modified titanium dioxide improves bonding strength and reduces residual matting agent content in the spinning solution, enabling efficient recycling and cost savings.

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Abstract

A matting-modified cellulose fiber includes a matting agent. The matting agent has a modified titanium dioxide. The modified titanium dioxide is functionalized with a functional group. The functional group of the modified titanium dioxide forms bonding with cellulose of the cellulose fiber. A method for manufacturing the matting-modified cellulose fiber includes the following steps: adding and mixing the cellulose and the matting agent into a spinning solution; forming a modified titanium dioxide by a surface modifier of the matting agent in the spinning solution activating and providing a functional group to a surface of the titanium dioxide , wherein the functional group of the modified titanium dioxide forms bonding with the cellulose; and manufacturing the matting-modified cellulose fiber through spinning the spinning solution based on the bonding between the modified titanium dioxide and the cellulose.
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Description

BACKGROUND OF THE INVENTION Technical Field

[0001] The present invention relates generally to the technology of cellulose fibers, and more particularly to a matting-modified or full dull cellulose fiber and method for manufacturing the same.Description of Related Art

[0002] Conventionally processes for producing regenerated cellulosic fiber (Lyocell) include dissolving a cellulose pulp in a spinning solvent (N-Methylmorpholine N-oxide, NMMO) filtering the cellulose pulp, and extruding the cellulose pulp through a spinneret to form the regenerated cellulosic fiber. Usually, the regenerated cellulosic fiber has a silk-like luster and is mainly used in textile products. In the non-textile field, the luster surface of the regenerated cellulosic fiber is not widely accepted.

[0003] In order to resolve the problem of the luster surface of the regenerated cellulosic fiber, a matte regenerated cellulosic fiber has been developed, wherein a matting agent and the cellulose pulp are added into the spinning solvent (NMMO) prior to spinning during the fiber processing. Because a traditional matting agent lacks a functional group for modifying a surface, the matting agent is coated on a surface of the regenerated cellulosic fiber by physical combination, thereby achieving the effect of reducing the luster of the regenerated cellulosic fiber.

[0004] However, when the cellulose pulp and the matting agent are mixed in the spinning solvent, the matting agent is dispersed and is merely adhered to a surface of the cellulose pulp without effectively forming a chemical bonding, so that the adhesion rate of the matting agent coated on the regenerated cellulosic fiber is affected. Additionally, after the regenerated cellulosic fiber is produced, a significant amount of the matting agent is remained in the spinning solvent, so that the spinning solvent cannot be recycled, thereby increasing the costs of the fiber processing.BRIEF SUMMARY OF THE INVENTION

[0005] In view of the above, the primary objective of the present invention is to provide a matting-modified cellulose fiber and a method for manufacturing the same, wherein the method enhances the recyclability of a spinning solution by using a matting agent of a modified titanium dioxide bonding with the matting-modified cellulose fiber.

[0006] The present invention provides a matting-modified cellulose fiber, including a matting agent, wherein the matting agent has a modified titanium dioxide; the modified titanium dioxide is functionalized with a functional group; the functional group of the modified titanium dioxide forms a bond with cellulose of the matting-modified cellulose fiber.

[0007] In an embodiment, the functional group of the modified titanium dioxide is selected from a group consisting of alkyl group, carboxyl group, alkenyl group, phenyl group, cycloalkyl group, ether group, ester group, aldehyde group, ketone group, amide group, amine group, thioether group, haloalkyl group, carbonate ester group, disulfide group, imine group, imide group, and sulfoxide group.

[0008] In an embodiment, a content of the matting agent bonding with the matting-modified cellulose fiber accounts for between 0.1wt% and 5wt% of an overall weight of the matting-modified cellulose fiber.

[0009] In an embodiment, the content of the matting agent bonding with the matting-modified cellulose fiber accounts for between 0.3wt% and 3wt% of the overall weight of the matting-modified cellulose fiber.

[0010] In an embodiment, a particle size distribution of the modified titanium dioxide is between 0.3µm and 1.5µm.

[0011] In an embodiment, the matting-modified cellulose fiber is selected from a group consisting of a long-fiber type and a short-fiber type.

[0012] The present invention further provides a method for manufacturing a matting-modified cellulose fiber includes the following steps. Step S1: adding and mixing cellulose and a matting agent into a spinning solution, wherein the matting agent comprises titanium dioxide and a surface modifier. Step S2: forming a modified titanium dioxide by the surface modifier in the spinning solution activating and providing a functional group to a surface of the titanium dioxide under a reaction condition of the spinning solution, wherein the functional group of the modified titanium dioxide forms bonding with the cellulose. Step S3: manufacturing the matting-modified cellulose fiber through spinning the spinning solution based on the bonding between the modified titanium dioxide and the cellulose.

[0013] In an embodiment, the spinning solution is an ionic liquid, a content of the matting agent in the spinning solution accounts for between 0.1wt% and 5wt% of an overall weight of the cellulose, a content of the cellulose accounts for between 5wt% and 30wt% of an overall weight of the spinning solution.

[0014] In an embodiment, the content of the matting agent in the spinning solution accounts for between 0.3wt% and 3wt% of the overall weight of the cellulose.

[0015] In an embodiment, the reaction condition of the spinning solution includes a reaction temperature ranging from 50°C to 180°C and a reaction time ranging from 0 hour to 12 hour, a particle size distribution of the modified titanium dioxide is between 0.3µm and 1.5µm.

[0016] In an embodiment, the functional group of the modified titanium dioxide is selected from a group consisting of alkyl group, carboxyl group, alkenyl group, phenyl group, cycloalkyl group, ether group, ester group, aldehyde group, ketone group, amide group, amine group, thioether group, haloalkyl group, carbonate ester group, disulfide group, imine group, imide group, and sulfoxide group.

[0017] In an embodiment, a content of the matting agent bonding with the matting-modified cellulose fiber accounts for between 0.1wt% and 5wt% of an overall weight of the matting-modified cellulose fiber, and the matting-modified cellulose fiber is selected from a group consisting of a long-fiber type and a short-fiber type.

[0018] In an embodiment, the spinning solution is recycled after the matting-modified cellulose fiber is manufactured, a residual content of the matting agent in the recycled spinning solution accounts for less than 0.5wt% of an overall weight of the recycled spinning solution.

[0019] With the aforementioned design, the matting-modified cellulose fiber of the present invention enhances a bonding strength of the matting agent with the matting-modified cellulose fiber by the modified titanium dioxide of the matting agent bonding with the matting-modified cellulose fiber. The residual content of the matting agent in the spinning solution could be effectively reduced in the method for manufacturing the matting-modified cellulose fiber, so that the recyclability of the spinning solution could be enhanced, thereby achieving the propose of saving the production cost.BRIEF DESCRIPTION OF THE SEVERAL VIEWS OF THE DRAWINGS

[0020] The present invention will be best understood by referring to the following detailed description of some illustrative embodiments in conjunction with the accompanying drawings, in which FIG. 1 is a micrograph of the matting-modified cellulose fiber according to an embodiment of the present invention; FIG. 2 is a particle size distribution graph of the modified titanium dioxide of the matting-modified cellulose fiber according to the embodiment of the present invention; and FIG. 3 is a flowchart, showing the method for manufacturing the matting-modified cellulose fiber according to another embodiment of the present invention. DETAILED DESCRIPTION OF THE INVENTION

[0021] A matting-modified cellulose fiber according to an embodiment of the present invention includes a matting agent. The matting agent has a modified titanium dioxide. The modified titanium dioxide is functionalized with a functional group, and the functional group of the modified titanium dioxide forms bonding with cellulose of the matting-modified cellulose fiber. The matting-modified cellulose fiber is selected from a group consisting of a long-fiber type and a short-fiber type. In other words, the matting-modified cellulose fiber could be the long-fiber type or the short-fiber type. The functional group of the modified titanium dioxide is selected from a group consisting of alkyl group, carboxyl group, alkenyl group, phenyl group, cycloalkyl group, ether group, ester group, aldehyde group, ketone group, amide group, amine group, thioether group, haloalkyl group, carbonate ester group, disulfide group, imine group, imide group, and sulfoxide group. A content of the matting agent bonding with the matting-modified cellulose fiber accounts for between 0.1wt% and 5wt% of an overall weight of the matting-modified cellulose fiber. In the current embodiment, the content of the matting agent bonding with the matting-modified cellulose fiber accounts for between 0.3wt% and 3wt% of the overall weight of the matting-modified cellulose fiber.

[0022] As illustrated in FIG. 1 and FIG. 2, the morphology of the modified titanium dioxide in the embodiment could be observed by using a scanning electron microscope (SEM), and a particle size distribution of the modified titanium dioxide is between 0.3µm and 1.5µm, wherein the particle size distribution of the modified titanium dioxide is concentrated in a range from 0.4µm to 1.0µm.

[0023] As illustrated in FIG. 3, a method for manufacturing the matting-modified cellulose fiber according to another embodiment of the present invention comprises the following steps:

[0024] Step S1: adding and mixing the cellulose and the matting agent into a spinning solution, wherein the spinning solution is an ionic liquid, and a content of the cellulose accounts for between 5wt% and 30wt% of an overall weight of the spinning solution. In the current embodiment, the ionic liquid can be a 40% to 60% NMMO aqueous solution, but not limited thereto. In an embodiment, the content of the cellulose accounts for between 8wt% and 20wt% of the overall weight of the spinning solution. The matting agent includes titanium dioxide and a surface modifier. In the current embodiment, the surface modifier is selected from a group consisting of carboxylic acid, alkyl isocyanate, ethoxysilane, methyl orthosilicate, silicon hydroxide, oyl halide, alkyl isothiocyanate, alkyl nitrite, nitroso, and alkyl thiocyanate; a content of the matting agent in the spinning solution accounts for between 0.1wt% and 5wt% of an overall weight of the cellulose. In an embodiment, the content of the matting agent in the spinning solution accounts for between 0.3wt% and 3wt% of the overall weight of the cellulose.

[0025] Step S2: forming a modified titanium dioxide by the surface modifier in the spinning solution activating and providing a functional group to a surface of the titanium dioxide under a reaction condition of the spinning solution, wherein the functional group of the modified titanium dioxide forms bonding with the cellulose. The reaction condition of the spinning solution includes a reaction temperature ranging from 50°C to 180°C and a reaction time ranging from 0 hour to 12 hour. More specifically, when the surface modifier is alkyl carboxylic acid, carboxyl group of the alkyl carboxylic acid reacts with an active site of a surface of the titanium dioxide to form a covalent bond, so that a structure of the surface of titanium dioxide is changed and a functional group of the alkyl carboxylic acid is modified to form the modified titanium dioxide, thereby enhancing a hydrophilicity of the modified titanium dioxide. Then the functional group of the alkyl carboxylic acid of the modified titanium dioxide reacts with a hydroxyl group of the cellulose to form bonding, thereby improving interfacial properties between the modified titanium dioxide and the cellulose.

[0026] Step S3: manufacturing the matting-modified cellulose fiber through spinning the spinning solution based on the bonding between the modified titanium dioxide and the cellulose, wherein a content of the matting agent bonding with the matting-modified cellulose fiber accounts for between 0.1wt% and 5wt% of an overall weight of the matting-modified cellulose fiber. In the current embodiment, the content of the modified titanium dioxide bonding with the matting-modified cellulose fiber accounts for between 0.3wt% and 3wt% of the overall weight of the matting-modified cellulose fiber. The spinning solution is recycled after the matting-modified cellulose fiber is manufactured, a residual content of the matting agent in the recycled spinning solution accounts for less than 0.5wt% of an overall weight of the recycled spinning solution. Therefore, the residual content of the matting agent in the recycled spinning solution is closed to 0wt%, indicating that almost all of the matting agent is combined with the matting-modified cellulose fiber. In this way, the residual content of the matting agent in the recycled spinning solution is relatively reduced, so that the spinning solution could be recycled.

[0027] In order to thoroughly illustrate the primary objective, features, and functions of the present invention, the current experiment provides property analyses of the matting-modified cellulose fiber, and experimental groups 1 to 4 are provided and are subjected to physical property tests.

[0028] The physical property tests of the experimental groups include the following steps: Step S1: adding and mixing the cellulose and the matting agent into the spinning solution, wherein the content of the matting agent in the spinning solution accounts for between 0.3wt% and 3wt% of the overall weight of the cellulose. In the current embodiment, the content of the matting agent in the spinning solution accounts for between 0.8wt% and 1.0wt% of the overall weight of the cellulose. Step S2: forming the modified titanium dioxide by the surface modifier in the spinning solution, wherein the modified titanium dioxide forms bonding with the cellulose. Step S3: manufacturing the matting-modified cellulose fiber with different deniers (D) through spinning the spinning solution based on the bonding between the modified titanium dioxide and the cellulose. The matting-modified cellulose fiber of the experimental group 1 has a denier of 134.45, the matting-modified cellulose fiber of the experimental group 2 has a denier of 133.94, the matting-modified cellulose fiber of the experimental group 3 has a denier of 128.11, and the matting-modified cellulose fiber of the experimental group 4 has a denier of 128.99. The experimental groups 1 to 4 are subjected to the physical property tests. Table 1: the results of the physical property tests of the experimental groups 1 to 4: ItemElongation rateTenacity strengthElastic modulus (Young's modulus 0.5-1%)Elastic modulus (Young's modulus 0.5-2%)Oil pick-up (%)Water pick-up (%)NMMO (%)Average (%)Coefficie nt of variation (CV%)Average (g / D)Coefficie nt of variation (CV%)Average (g / D)Average (g / D)Experimental group 16.143.953.651.66141.9782.20.78413.2841.257Experimental group 26.037.783.474.01130.1477.440.88614.3051.339Experimental group 35.464.983.621.93156.5393.260.77612.8251.169Experimental group 45.9611.113.535.44143.4384.770.80514.0551.216

[0029] It could be seen from Table 1 that roving yarns with a denier ranging from 20 to 400 manufactured from the matting-modified cellulose fibers of the experimental groups 1 to 4 have an excellent performance of elongation rate and elastic coefficient, and the matting-modified cellulose fibers of the experimental groups 1 to 4 are matte.

[0030] Next, binding contents of the matting agent in the experimental groups 1 to 4 and the residual content of the matting agent in the recycled spinning solution are explored.

[0031] The binding contents of the matting agent in the matting-modified cellulose fiber is measured by using Inductively Coupled Plasma-Optical Emission Spectrometer (ICP-OES), wherein the detection limit of the ICP-OES is 2 mg / kg, which is equivalent to less than 0.0004wt%. In other words, when the binding contents of the matting agent in the matting-modified cellulose fiber is less than 0.0004wt%, the ICP-OES could not detect the matting agent. As the preparation conditions and the compositions of the experimental groups 1 to 4 are the same, the experimental group 1 is selected for measuring the binding contents of the matting agent in the matting-modified cellulose fiber. The result shows the binding contents of the matting agent in the matting-modified cellulose fiber of the experimental group 1 in the current experiment is 0.8276wt%. Additionally, the residual content of the matting agent in the recycled spinning solution is measured. Similarly, the ICP-OES is used to analyze the residual content of the matting agent in the recycled spinning solution of the experimental group 1. The result shows that the ICP-OES does not detect the residual content of the matting agent in the recycled spinning solution of the experimental group 1, so that the residual content of the matting agent in the recycled spinning solution of the experimental group 1 is less than 0.0004wt%, even approaching to 0wt%. Therefore, the current experiment proves that almost all of the matting agent is combined with the matting-modified cellulose fiber, and the residual content of the matting agent in the recycled spinning solution is greatly reduced, so that the recycled spinning solution could be reused.

[0032] In summary, the matting-modified cellulose fiber of the current experiment enhances a bonding strength of the matting agent with the matting-modified cellulose fiber by the modified titanium dioxide of the matting agent bonding with the matting-modified cellulose fiber. The residual content of the matting agent in the spinning solution could be effectively reduced in the method for manufacturing the matting-modified cellulose fiber, so that the recyclability of the spinning solution could be enhanced, thereby achieving the propose of saving the production cost.

Claims

1. A matting-modified cellulose fiber, comprising a matting agent, wherein the matting agent has a modified titanium dioxide; the modified titanium dioxide is functionalized with a functional group; the functional group of the modified titanium dioxide forms bonding with cellulose of the cellulose fiber.

2. The matting-modified cellulose fiber as claimed in claim 1, wherein the functional group of the modified titanium dioxide is selected from a group consisting of alkyl group, carboxyl group, alkenyl group, phenyl group, cycloalkyl group, ether group, ester group, aldehyde group, ketone group, amide group, amine group, thioether group, haloalkyl group, carbonate ester group, disulfide group, imine group, imide group, and sulfoxide group.

3. The matting-modified cellulose fiber as claimed in claim 1 or 2, wherein a content of the matting agent bonding with the matting-modified cellulose fiber accounts for between 0.1wt% and 5wt% of an overall weight of the matting-modified cellulose fiber.

4. The matting-modified cellulose fiber as claimed in claim 3, wherein the content of the matting agent bonding with the matting-modified cellulose fiber accounts for between 0.3wt% and 3wt% of the overall weight of the matting-modified cellulose fiber.

5. The matting-modified cellulose fiber as claimed in claim 3, wherein a particle size distribution of the modified titanium dioxide is between 0.3µm and 1.5µm.

6. The matting-modified cellulose fiber as claimed in claim 1, wherein the matting-modified cellulose fiber is selected from a group consisting of a long-fiber type and a short-fiber type.

7. A method for manufacturing a matting-modified cellulose fiber, comprising: step S1: adding and mixing cellulose and a matting agent into a spinning solution, wherein the matting agent comprises titanium dioxide and a surface modifier; step S2: forming a modified titanium dioxide by the surface modifier in the spinning solution activating and providing a functional group to a surface of the titanium dioxide under a reaction condition of the spinning solution, wherein the functional group of the modified titanium dioxide forms bonding with the cellulose; and step S3: manufacturing the matting-modified cellulose fiber through spinning the spinning solution based on the bonding between the modified titanium dioxide and the cellulose.

8. The method as claimed in claim 7, wherein in step S1, the surface modifier is selected from a group consisting of carboxylic acid, alkyl isocyanate, ethoxysilane, methyl orthosilicate, silicon hydroxide, oyl halide, alkyl isothiocyanate, alkyl nitrite, nitroso, and alkyl thiocyanate.

9. The method as claimed in claim 7 or 8, wherein in step S1, the spinning solution is an ionic liquid; a content of the matting agent in the spinning solution accounts for between 0.1wt% and 5wt% of an overall weight of the cellulose; a content of the cellulose accounts for between 5wt% and 30wt% of an overall weight of the spinning solution.

10. The method as claimed in claim 9, wherein the content of the matting agent in the spinning solution accounts for between 0.3wt% and 3wt% of the overall weight of the cellulose.

11. The method as claimed in claim 9, wherein in step S2, the reaction condition of the spinning solution includes a reaction temperature ranging from 50°C to 180°C and a reaction time ranging from 0 hour to 12 hour; a particle size distribution of the modified titanium dioxide is between 0.3µm and 1.5µm.

12. The method as claimed in claim 7, wherein the functional group of the modified titanium dioxide is selected from a group consisting of alkyl group, carboxyl group, alkenyl group, phenyl group, cycloalkyl group, ether group, ester group, aldehyde group, ketone group, amide group, amine group, thioether group, haloalkyl group, carbonate ester group, disulfide group, imine group, imide group, and sulfoxide group.

13. The method as claimed in claim 11, wherein in step S3, a content of the matting agent bonding with the matting-modified cellulose fiber accounts for between 0.1wt% and 5wt% of an overall weight of the matting-modified cellulose fiber, and the matting-modified cellulose fiber is selected from a group consisting of a long-fiber type and a short-fiber type.

14. The method as claimed in claim 13, wherein in step S3, the spinning solution is recycled after the matting-modified cellulose fiber is manufactured; a residual content of the matting agent in the recycled spinning solution accounts for less than 0.5wt% of an overall weight of the recycled spinning solution.

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