Delustering modified cellulose fiber and manufacturing method thereof
By introducing modified titanium dioxide into cellulose rayon and forming a bond with cellulose, the problems of low matting agent adhesion rate and large residual amount are solved, and efficient bonding of the matting agent and recycling of the spinning solution are achieved.
Patent Information
- Application Number
- CN202410279502.6
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2024-03-12
- Publication Date
- 2025-09-16
AI Technical Summary
Existing cellulose man-made fibers cannot effectively form bonds during the matting agent mixing process, resulting in low matting agent adhesion rate and large amount of spinning solution residue, which increases process costs.
Modified titanium dioxide is used as a matting agent, and functional groups are modified in the spinning solution to form bonds with cellulose, thereby enhancing the bonding strength and reducing the residual amount.
By modifying the bond between titanium dioxide and cellulose, the adhesion rate of the matting agent is increased and the residual amount in the spinning solution is significantly reduced, saving process costs.
Smart Images
Figure CN120649175A_ABST
Abstract
Description
Technical Field
[0001] The present invention relates to the technology of cellulose fibers, and in particular to a modified cellulose fiber with dull or matte finish and a method for manufacturing the same. Background Art
[0002] The known process for producing cellulose rayon (Lyocell) involves dissolving cellulose slurry in a spinning solvent (NMMO), filtering and squeezing the cellulose slurry through a spinning nozzle to form the fibers. Lyocell fibers typically have a silky sheen and are primarily used in the textile market. However, in the non-textile sector, the glossy surface of lyocell fibers is less readily accepted by the market.
[0003] To improve the glossy surface of cellulose fibers, relevant industry players have developed matte cellulose fibers. During the fiber production process, cellulose pulp and a matting agent are added to a spinning solvent (NMMO) for spinning. Because traditional matting agents lack surface-modifying functional groups, the matting agent coats the surface of the cellulose fibers, forming a physical bond with the fibers and reducing their brightness and gloss.
[0004] However, during the mixing process of the cellulose pulp and the matting agent, the matting agent can only be dispersed and attached to the surface of the cellulose pulp and cannot effectively form a bonding effect, thereby affecting the adhesion rate of the matting agent coated on the cellulose rayon. In addition, after the cellulose rayon process, a large amount of the matting agent remains in the spinning solution, making it impossible to recover the spinning solution, resulting in increased fiber process costs. Summary of the Invention
[0005] In view of this, the object of the present invention is to provide a matte modified cellulose fiber and a method for manufacturing the same, which improves the effect of recovering process solution by generating bonding ability between the matte modification and the cellulose fiber.
[0006] To achieve the above objectives, the present invention provides a matting modified cellulose fiber comprising a matting agent having a modified titanium dioxide modified with a functional group to form a bond with the cellulose in the cellulose fiber.
[0007] In one embodiment, the functional group comprises one of the group consisting of alkyl, alkenyl, olefin, phenyl, cycloalkyl, ether, ester, aldehyde, ketone, amide, amino, sulfide, haloalkyl, carbonate, disulfide, imine, amide, and sulfoxide.
[0008] In one embodiment, the matting agent is incorporated into the cellulose fibers in an amount ranging from 0.1 to 5 wt %.
[0009] In one embodiment, the matting agent is incorporated into the cellulose fibers in an amount ranging from 0.3 to 3 wt %.
[0010] In one embodiment, the particle size distribution of the modified titanium dioxide is between 0.3 μm and 1.5 μm.
[0011] In one embodiment, the cellulose fibers include one of long fiber form and short fiber form.
[0012] Another embodiment of the present invention provides a method for producing matte-modified cellulose fibers, comprising the following steps: Step S1, adding cellulose and a matting agent to a spinning solution for mixing, wherein the matting agent comprises titanium dioxide and a surface modifier; Step S2, subjecting the spinning solution to reaction conditions, wherein the surface modifier activates the titanium dioxide surface to modify it with a functional group, thereby forming modified titanium dioxide, wherein the functional group of the modified titanium dioxide forms a bond with the cellulose; and Step S3, spinning the cellulose fibers to produce the cellulose fibers based on the bond between the modified titanium dioxide and the cellulose.
[0013] In one embodiment, the spinning solution is an ionic liquid, the content of the matting agent is 0.1-5 wt % of the total weight of the cellulose, and the content of the cellulose is 5-30 wt % of the total weight of the spinning solution.
[0014] In one embodiment, the content of the matting agent is 0.3-3 wt % based on the total weight of the cellulose.
[0015] In one embodiment, the reaction conditions of the spinning solution include a reaction temperature of 50° C. to 180° C., a reaction time of 0 to 12 hours, and a particle size distribution of the modified titanium dioxide is between 0.3 μm and 1.5 μm.
[0016] In one embodiment, the functional groups modified by the modified titanium dioxide include one of the group consisting of alkyl, alkenyl, olefin, phenyl, cycloalkyl, ether, ester, aldehyde, ketone, amide, amino, sulfide, haloalkyl, carbonate, disulfide, imine, amide and sulfoxide.
[0017] In one embodiment, the modified titanium dioxide is combined with the cellulose fibers in an amount ranging from 0.1 to 5 wt %, and the cellulose fibers are in a long fiber form and a short fiber form.
[0018] In one embodiment, the spinning solution is recovered after the cellulose fiber is produced, and the residual amount of the matting agent in the recovered spinning solution is less than 0.5 wt %.
[0019] The present invention provides a matting modified cellulose fiber. The modified titanium dioxide in the matting agent forms a bond with the cellulose fiber, thereby enhancing the bonding strength between the matting agent and the cellulose fiber. Furthermore, the residual content of the matting agent in the spinning solution during the process is effectively reduced, thereby improving the recovery efficiency of the spinning solution and achieving the goal of saving process costs. BRIEF DESCRIPTION OF THE DRAWINGS
[0020] Figure 1 This is a microscopic image of modified titanium dioxide in matte modified cellulose fibers according to a preferred embodiment.
[0021] Figure 2 FIG1 is a particle size distribution diagram of modified titanium dioxide in matte modified cellulose fibers according to a preferred embodiment.
[0022] Figure 3 FIG1 is a flow chart of the steps of modifying cellulose fibers with matte finish according to a preferred embodiment.
[0023] Description of reference numerals:
[0024] S1~S3:Steps DETAILED DESCRIPTION
[0025] A preferred embodiment of the present invention provides a modified cellulose fiber with matting properties, comprising a matting agent comprising modified titanium dioxide modified with a functional group that forms a bond with cellulose in the cellulose fiber. The cellulose fiber comprises either a long fiber form or a short fiber form, meaning the cellulose fiber can be suitable for either a long fiber form or a short fiber form. The functional group of the modified titanium dioxide comprises one of the group consisting of an alkyl group, an alkenyl group, an olefin group, a phenyl group, a cycloalkyl group, an ether group, an ester group, an aldehyde group, a ketone group, an amide group, an amino group, a sulfide group, a haloalkyl group, a carbonate group, a disulfide group, an imide group, an amide group, and a sulfoxide group. The matting agent is bound to the cellulose fiber at a content of 0.1 to 5 wt%. In a preferred embodiment, the matting agent is bound to the cellulose fiber at a content of 0.3 to 3 wt%.
[0026] like Figure 1 、 Figure 2 As shown, the morphology of the modified titanium dioxide described in the embodiment can be observed by scanning electron microscopy, and the particle size distribution of the modified titanium dioxide is between 0.3 and 1.5 μm, wherein the particle size distribution of the modified titanium dioxide is concentrated in the range of 0.4 to 1.0 μm.
[0027] like Figure 3 As shown, another embodiment of the present invention provides a method for producing matte modified cellulose fibers, which comprises the following steps:
[0028] In step S1, cellulose and the matting agent are added to a spinning solution and mixed. The spinning solution is an ionic liquid, and the content of the cellulose accounts for 5-30 wt% of the total weight of the spinning solution. In this embodiment, the ionic liquid may be a 40-60% aqueous solution of N-methylmorpholine N-oxide (NMMO), but is not limited thereto. In a preferred embodiment, the content of the cellulose accounts for 8-20 wt% of the total weight of the spinning solution. The matting agent comprises titanium dioxide and a surface modifier. In this embodiment, the surface modifier comprises carboxylic acid, alkyl isocyanate, ethoxysilane, methyl orthosilicate, silicon hydroxide, oylhalide, alkyl isothiocyanate, alkyl nitrite, nitroso compound, alkyl thiocyanate, and alkyl thiocyanate. The matting agent is one of the group consisting of thiocyanate, and the content of the matting agent is 0.1-5wt% of the total weight of the cellulose. In a preferred embodiment, the content of the matting agent is 0.3-3wt% of the total weight of the cellulose.
[0029] In step S2, the spinning solution is subjected to a reaction condition in which the surface modifier activates the surface of the titanium dioxide to modify the functional group to form the modified titanium dioxide, and the functional group of the modified titanium dioxide forms a bond with the cellulose, wherein the reaction conditions of the spinning solution include a reaction temperature of 50°C to 180°C and a reaction time of 0 to 12 hours. More specifically, when the surface modifier is an alkyl carboxylic acid, the carboxyl group (COOH) in the alkyl carboxylic acid reacts with the active site on the surface of the titanium dioxide to form a covalent bond, thereby changing the structure of the titanium dioxide surface and modifying the functional group of the alkyl carboxyl group to form the modified titanium dioxide, so as to enhance the hydrophilicity of the modified titanium dioxide. Then, the modified titanium dioxide reacts and bonds with the hydroxyl functional group of the cellulose through the functional group of the alkyl carboxyl group, thereby improving the interfacial properties between titanium dioxide and cellulose.
[0030] In step S3, the modified titanium dioxide reacts with the cellulose to form bonds, and the spinning solution is processed to produce the cellulose fibers. The modified titanium dioxide is bound to the cellulose fibers in an amount ranging from 0.3 to 3 wt %. After the cellulose fibers are produced, the spinning solution is recovered. The residual amount of the matting agent in the recovered spinning solution is less than 0.5 wt %. Therefore, the residual amount of the matting agent in the recovered spinning solution can be close to 0 wt %, indicating that the matting agent is nearly completely bound to the cellulose fibers, thereby relatively reducing the residual amount of the matting agent in the spinning solution and achieving the effect of recycling the spinning solution.
[0031] In addition, in order to fully understand the purpose, features and technical effects of the present invention, this embodiment provides a property analysis of the matte modified cellulose fiber, and this experiment provides an experimental group for physical property testing.
[0032] Experimental group test steps:
[0033] Step S1, adding cellulose and the matting agent into the spinning solution and mixing them, wherein the content of the matting agent accounts for 0.3-3 wt% of the total weight of the cellulose. In this embodiment, the content of the matting agent accounts for 0.8-1.0 wt% of the total weight of the cellulose.
[0034] In step S2, the matting agent reacts with the spinning solution to form the modified titanium dioxide, and the modified titanium dioxide forms a bond with the cellulose.
[0035] Step S3, processing the spinning solution to produce the cellulose fibers of different deniers (D), wherein this experiment includes experimental group 1 having a cellulose fiber with a denier of 134.45, experimental group 2 having a cellulose fiber with a denier of 133.94, experimental group 3 having a cellulose fiber with a denier of 128.11, and experimental group 4 having a cellulose fiber with a denier of 128.99, and the experimental groups 1 to 4 are respectively subjected to physical property tests.
[0036] Table 1. Physical properties of cellulose fibers in experimental groups 1 to 4:
[0037]
[0038] According to the results in Table 1, the cellulose fibers were processed into coarse yarns with a denier of 20-400, wherein the experimental groups 1 to 4 had excellent elongation and elastic modulus, and the experimental groups 1 to 4 all had matte properties.
[0039] Next, the combined amount of the matting agent in the experimental groups 1 to 4 and the residual amount of the matting agent in the recovered spinning solution were investigated.
[0040] In this test, the amount of matting agent in the cellulose fiber is detected by inductively coupled plasma-optical emission spectrometry (ICP-OES), wherein the detection limit of the ICP-OES device is 2 mg / kg, which is equivalent to less than 0.0004 wt%. That is, when the matting agent content is less than 0.0004 wt%, it means that the matting agent is not detected. Since the preparation conditions and compositions of experimental groups 1 to 4 are the same, experimental group 1 is selected in this test to detect the content of the matting agent in the cellulose fiber. In this embodiment, the test results of experimental group 1 show that the amount of matting agent in the cellulose fiber is 0.8276%. In addition, the recovered spinning solution The residual amount of the matting agent was also tested using inductively coupled plasma-optical emission spectroscopy (ICP-OES) analysis in the recovered spinning solution of Experimental Group 1. The test results showed that the residual amount of the matting agent (modified titanium dioxide) in the recovered spinning solution of Experimental Group 1 was not detected, indicating that the residual amount of the matting agent (modified titanium dioxide) in the recovered spinning solution of Experimental Group 1 was less than 0.0004 wt %, and even close to 0 wt %. This confirms that the content of the matting agent in this example is indeed almost completely bound to the cellulose fibers, and significantly reduces the residual amount of the matting agent in the recovered spinning solution, allowing the recovered spinning solution to be reused.
[0041] In summary, the matting modified cellulose fibers described in this embodiment are characterized by the modified titanium dioxide in the matting agent forming a bond with the cellulose fibers, thereby enhancing the bonding strength between the matting agent and the cellulose fibers. Furthermore, the residual content of the matting agent in the spinning solution during the process can be effectively reduced, thereby improving the recovery efficiency of the spinning solution and achieving the goal of saving process costs.
[0042] The above description is only a preferred embodiment of the present invention. Any equivalent changes made by applying the description and claims of the present invention should be included in the patent scope of the present invention.
Claims
1. A matting modified cellulose fiber, comprising a matting agent, wherein the matting agent comprises a modified titanium dioxide, wherein the modified titanium dioxide is modified with a functional group to form a bond with cellulose in the cellulose fiber.
2. The matte-finished modified cellulose fiber according to claim 1, wherein the functional group comprises one of the group consisting of an alkyl group, an alkenyl group, an olefin group, a phenyl group, a cycloalkyl group, an ether group, an ester group, an aldehyde group, a ketone group, an amide group, an amino group, a sulfide group, a haloalkyl group, a carbonate group, a disulfide group, an imine group, an imido group, and a sulfoxide group.
3. The matte modified cellulose fiber according to claim 1 or 2, wherein the matting agent is incorporated into the cellulose fiber in an amount ranging from 0.1 to 5 wt%.
4. The matte modified cellulose fiber according to claim 3, wherein the matting agent is incorporated into the cellulose fiber in an amount ranging from 0.3 to 3 wt%. 5 . The matte modified cellulose fiber according to claim 3 , wherein the particle size distribution of the modified titanium dioxide is between 0.3 and 1.5 μm. 6 . The matte modified cellulose fiber according to claim 1 , wherein the cellulose fiber comprises a long fiber form and a short fiber form.
7. A method for producing matte modified cellulose fibers, comprising the following steps: Step S1, adding cellulose and a matting agent into a spinning solution and mixing them, wherein the matting agent comprises titanium dioxide and a surface modifier; Step S2, the spinning solution is subjected to a reaction condition, the surface modifier activates the surface of the titanium dioxide to modify a functional group, thereby forming a modified titanium dioxide, and the functional group of the modified titanium dioxide forms a bond with the cellulose; as well as Step S3: producing the cellulose fiber by spinning based on the bonding of the modified titanium dioxide and the cellulose.
8. The method for producing matte-modified cellulose fibers according to claim 7, wherein in step S1, the surface modifier comprises one of the group consisting of carboxylic acid, methyl isocyanate, ethoxysilane, methyl orthosilicate, silicon hydroxide, acyl chloride, alkyl isothiocyanate, alkyl nitrite, nitroso compound, and thiocyanate.
9. The method for producing matt modified cellulose fibers according to claim 7 or 8, wherein in step S1, the spinning solution is an ionic liquid, the content of the matting agent is 0.1-5 wt% of the total weight of the cellulose, and the content of the cellulose is 5-30 wt% of the total weight of the spinning solution.
10. The method for producing matt modified cellulose fibers according to claim 9, wherein the content of the matting agent is 0.3-3 wt% based on the total weight of the cellulose.
11. The method for producing matte modified cellulose fibers according to claim 9, wherein in step S2, the reaction conditions of the spinning solution include a reaction temperature of 50°C to 180°C, a reaction time of 0 to 12 hours, and a particle size distribution of the modified titanium dioxide ranging from 0.3 to 1.5 μm.
12. The method for producing matte modified cellulose fibers according to claim 7, wherein the functional groups modified by the modified titanium dioxide include one of the group consisting of alkyl, alkenyl, olefin, phenyl, cycloalkyl, ether, ester, aldehyde, ketone, amide, amino, sulfide, haloalkyl, carbonate, disulfide, imine, amide, and sulfoxide.
13. The method for producing matte modified cellulose fibers according to claim 11, wherein in step S3, the content of the modified titanium dioxide bonded to the cellulose fibers is between 0.1 and 5 wt%, and the cellulose fibers are in either a long fiber form or a short fiber form.
14. The method for producing matte modified cellulose fibers according to claim 13, wherein in step S3, the spinning solution is recovered after the cellulose fibers are produced, and the residual amount of the matting agent in the recovered spinning solution is less than 0.5 wt%.