Seaweed fiber and method for producing the same
A method using sodium alginate and five-membered ring quaternary amine salt polymer addresses the dyeing challenges of seaweed fibers, enabling stable and vivid coloration while preserving fiber strength.
Patent Information
- Authority / Receiving Office
- JP · JP
- Patent Type
- Patents
- Current Assignee / Owner
- Filing Date
- 2022-05-09
- Publication Date
- 2026-03-18
AI Technical Summary
Seaweed fibers are difficult to dye due to poor acid and alkali resistance, susceptibility to ammonium and sodium salts, and swelling or dissolution when exposed to ON solutions, which limits their application in the textile industry.
A manufacturing method involving a spinning solution with sodium alginate and a five-membered ring quaternary amine salt polymer, followed by coagulation, stretching, and immersion in a treatment agent, to create dyeable seaweed fibers with stable dyeing sites.
The method achieves high dyeing rates and colorfastness, maintaining the fibers' mechanical integrity and allowing vivid coloration without using salts, overcoming the limitations of previous dyeing techniques.
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Abstract
Description
[Technical Field]
[0001] This application belongs to the technical field of dyeing textiles, and more particularly to seaweed fibers and methods for producing them. [Background technology]
[0002] Seaweed fiber is made from sodium alginate extracted from natural seaweed and produced by a wet spinning method. It is a newly manufactured, environmentally friendly, biodegradable fiber. Seaweed fiber has excellent moisture absorption and film-forming properties. It is considered important due to its properties such as fibrousness, fibrousness, good biodegradability, and biocompatibility.
[0003] Seaweed fibers are now widely used in the field of medical dressings, as well as in high-end clothing and underwear. The fabric and decorative textiles show promising future potential.
[0004] The smooth texture of seaweed fibers makes them comfortable to wear, but also makes spinning them difficult. Meanwhile, related technologies... Therefore, achieving pure spinning of seaweed fibers is difficult. On the other hand, the price of seaweed fibers is still somewhat low. Because it is expensive, seaweed fiber blended fabrics are more common in the market.
[0005] Among these, there are two main varieties of blends: one made from seaweed fiber and cotton, and the other from seaweed fiber and wool. The blended fibers can also possess excellent wearability properties such as antibacterial and flame retardant properties, making them suitable for clothing. The industrial textile industry shows promising potential for future industrialization in both sectors.
[0006] However, seaweed fiber has poor acid and alkali resistance, and is susceptible to ammonium salts and sodium. + , K + H + stomach When it comes into contact with an ON solution, it swells or dissolves. For this reason, in current staining systems, seaweed Dyeing the fibers is difficult. The difficulty in dyeing seaweed fibers poses a problem for large-scale applications in the spinning industry. This is a bottleneck that limits its applications.
[0007] In related technologies, CN101736440A uses water-soluble dendrimers and alginate fibers. In addition to the spinning solution, a wet spinning apparatus and process are employed to perform coagulation, stretching, washing, and post-treatment. This document discloses a method for producing dyeable seaweed fibers, which involves performing this process to obtain dyeable seaweed fibers. In this method, it is important to add polyamide-amine dendrimer to the spinning solution, but sea The strong electronegativity of algal fibers could not be overcome, so salts had to be added to accelerate the dyeing process. Yes, and damage to the seaweed fibers cannot be avoided.
[0008] In addition, there is a paper published by Shao Huangxiang et al. on direct dye-free dyeing of calcium alginate fibers. (Printing, October 2014, 1-5) and the paper by Liu Jie et al. on the reaction of alginate fibers Research on dyeing techniques (printing technology, March 2014, pp. 11-13) is a method for producing seaweed fibers. This was reported. Both papers used calcium chloride, and the former was calcium chloride. The latter uses calcium chloride as a fixative, while the latter uses calcium chloride as an accelerator. This makes the fibers brittle and prone to breaking. Calcium chloride is used as an accelerator, and in the paper... As described, the strength loss is very large, decreasing by approximately 30-40%.
[0009] Even today, some salt-free cotton dyeing techniques are not suitable for dyeing seaweed fibers due to various limitations. It's not possible. As with CN108914630A, the caustic soda concentration of the pretreatment solution must be between 2 and 6. The concentration is g / L, and this process essentially dissolves the seaweed fibers. For example, CN106 As in 498770A, adsorbent cationic modifiers are used for cotton modification, and caustic soda is used. It is not used. However, obvious linear quaternary ammonium salt polymers have a low adsorption and cross-linking effect with seaweed fibers, swelling and dissolving the seaweed fibers, and adversely affecting the usability of the seaweed fibers. .
[0010] From the above, those skilled in the art need to find a manufacturing method that can solve the problem of difficult dyeing of seaweed fibers without destroying the morphological structure of the seaweed fibers and reducing the strength of the seaweed fibers. [[ID=I0]]It is urgent. [[ID=II]]
Summary of the Invention
Problems to be Solved by the Invention
Problems to be Solved by the Invention
[0011] This application aims to provide seaweed fibers and a manufacturing method thereof in order to solve the technical problems in the prior art that it is difficult to dye seaweed fibers.
Means for Solving the Problems
Means for Solving the Problems
[0012] In order to solve the above technical problems, this application is implemented as follows.
[0013] This application includes step S10 of manufacturing a spinning solution using a raw material containing sodium alginate, step S20 of extruding the spinning solution obtained in S10 into a coagulation bath for coagulation molding to obtain primary fibers, 0, and step S30 of stretching and washing with water the primary fibers obtained in S20 to obtain seaweed fibers, step S40 of immersing the seaweed fibers obtained in S30 in a treatment agent for post-treatment, and includes providing a manufacturing method of seaweed fibers, wherein at least any one or all of the raw material of S10, the coagulation bath of S20, and the treatment agent of S30 contain a 5 member ring quaternary amine salt polymer.
[0014] In addition, the technical solution according to the above embodiment of the present invention has the following additional technical features That's fine.
[0015] In the above technical solution, the five-membered ring quaternary amine salt polymer is as shown below. ru. TIFF0007832614000001.tif4355 (However, R1 is CH3, CH2CH3, CH2(CH2)4CH3, CH2(CH2 ) 10 CH3, CH2(CH2) 16 It is CH3 or C6H5CH2, and R2 is CH 3, CH2CH3, CH2(CH2)4CH3, CH2(CH2) 10 CH3, CH2 ( CH2) 16 It is CH3 or C6H5CH2, and the degree of polymerization n is in the range of 50 to 25000. be.)
[0016] In any of the above technical solutions, the content of the 5-membered ring quaternary amine salt polymer in the seaweed fiber The amount is between 0.1% by mass and 10% by mass.
[0017] In any of the above technical solutions, S10 specifically means: Sodium alginate: 5-membered ring quaternary amine salt polymer = 100: (0.001~30) Sodium alginate and a five-membered ring quaternary amine salt polymer are mixed in water in a mass ratio, and then spun. The process includes step S101, which involves obtaining a liquid.
[0018] In any of the above technical solutions, the concentration of sodium alginate in the spinning solution is 3 It is between 6% by mass.
[0019] In any of the above technical solutions, S20 specifically means: After the spinning solution obtained in S10 is allowed to stand and degassed, a 5-membered ring quaternary compound with a concentration of 0.01% to 2% by mass is obtained. The material is extruded into a coagulation bath at a temperature of 40°C to 70°C containing an amine salt polymer, and then coagulated and molded into primary fibers. The procedure includes step S201 to obtain the result.
[0020] And / or, in any of the above technical solutions, S40 specifically means The seaweed fibers obtained in S30 are immersed in a treatment agent at a temperature of 20-70°C for 5 min to 60 min. n includes step S401 of immersion treatment, The treatment agent contains 0.5% to 10% of five-membered ring quaternary granular It contains amine salt polymers.
[0021] In any of the above technical solutions, in S20, the pH of the coagulation bath is 4.5 to 6. The answer is 5.
[0022] In any of the above technical solutions, in S20, the coagulation bath has a concentration of 1% by mass. This is a 6% by mass aqueous solution of calcium chloride.
[0023] In any of the above technical solutions, after S40, the manufacturing method is: The step S50 further includes washing and drying the seaweed fibers obtained in S40. This application also relates to seaweed fibers obtained using the manufacturing method described in any of the above technical solutions. To provide maintenance. [Effects of the Invention]
[0024] The beneficial effects of this application are as follows: First, the method for producing seaweed fibers according to this invention has a high dyeing rate and a low loss rate of seaweed fibers, and soap It has high colorfastness against washing. Therefore, this invention makes it possible to obtain seaweed fibers with vivid colors. Cut. Furthermore, the method for producing seaweed fibers according to this invention does not destroy the morphological structure of the seaweed fibers, and is non-salt. It can be dyed using non-alkaline dyes and provides maximum protection for seaweed fibers. Finally, the method for producing seaweed fibers according to the present invention utilizes spinning crosslinking and post-finishing processes, and is appropriate By selecting raw materials, ratios, reaction conditions, etc., quaternary ammonia can be formed inside and on the surface of seaweed fibers. By constructing a nium-staining site and producing dyeable seaweed fibers, current seaweed fibers This solves the bottleneck in industrial applications. Additional aspects and advantages of the present application are partially shown in the following description, and are partially shown in the following description. This will become clear from the outset or will be understood through the practical application of this invention. [Brief explanation of the drawing]
[0025] [Figure 1] This is a scanning electron microscope image of seaweed fibers using conventional technology. [Figure 2] This is a scanning electron microscope image of seaweed fibers according to the present invention. [Modes for carrying out the invention]
[0026] The embodiments described below with reference to the drawings are illustrative examples used solely to illustrate the present application. This is not intended to limit the present application. Based on the embodiments of this application, a person skilled in the art can... All other embodiments obtained without requiring creative effort are within the scope of the present application.
[0027] The embodiments of the present application are methods for producing seaweed fibers, Step S10 involves preparing a spinning solution using a raw material containing sodium alginate, Step S2 involves extruding the spinning solution obtained in S10 into a coagulation bath and coagulating and shaping it to obtain primary fibers. 0 and, Step S30 involves stretching and washing the primary fibers obtained in S20 to obtain seaweed fibers, The process includes step S40, in which the seaweed fibers obtained in S30 are immersed in a treatment agent for post-treatment, At least one or all of the raw materials of S10, the coagulation bath of S20, and the treatment agent of S30 are 5 The present invention provides a method for producing seaweed fibers containing a quaternary amine salt polymer.
[0028] In the above embodiment, the seaweed fiber of the embodiment of the present application is used, along with one or two other materials. It is possible to manufacture seaweed fiber blended fabrics, which are blended fabrics with more than one species of fiber. For example, sea Algae fiber blended fabrics include seaweed fiber / cotton blended fabrics, seaweed fiber / viscose blended fabrics, and seaweed fiber... Wool blend fabrics, seaweed fiber / cashmere blend fabrics, seaweed fiber / silk blend fabrics at least One type is sufficient.
[0029] In the above embodiment, the seaweed fiber of the present invention is easy to dye and has a vivid color. Dyeing is performed using one or more of the following: dyes, acid dyes, reactive dyes, natural dyes, and indigo dyes. It is possible.
[0030] In the above example, at least the raw material of S10, the coagulation bath of S20, and the treatment agent of S30 The presence of any or all of a five-membered ring quaternary amine salt polymer is due to the adhesion of seaweed fibers during dyeing. To improve dyeing efficiency, reduce the loss rate of seaweed fibers, and improve the colorfastness of seaweed fibers against soap washing. This is to make it so. The seaweed fiber blended fabric obtained by the manufacturing method according to the embodiment of this application is The dye penetration rate is 85% or higher, and the colorfastness to soap washing is level 4 or higher.
[0031] The principle by which the embodiments of this application can achieve the above objective is as follows: Alginic acid Sodium is a block of two different uronic acids linked by a C-1,4 bond. It is a polysaccharide, namely, β-D-mannuronic acid (abbreviated as M unit) and α-L-guluronic acid (abbreviated as G unit). The two structural units in the sodium alginate molecule are polymer ic mannuronic acid (M)n and poly guluronic acid (G)n, which are distributed in the molecular chain in the form of mutual MG or multiple alternation (MG)n, and their chemical structure is as follows. TIFF0007832614000002.tif43146
[0032] When the sodium alginate spinning solution encounters a coagulation bath containing calcium chloride, the sodium alginate spinning solution rapidly changes into a water-insoluble calcium alginate gel. This process mainly makes the GG segment and Ca 2+ form an "egg-shell" structure to produce seaweed fibers. Many monovalent salts destroy the stability of seaweed fibers, that is, they destroy their "egg-shell" cross-linked structure .
[0033] One of the key points of this application is that at least any one or all of the raw material of S10, the coagulation bath of S20, and the treatment agent of S30 contain a five-membered ring quaternary ammonium salt polymer. By adding the five-membered ring quaternary ammonium salt polymer in different steps (one or more steps) of spinning, a quaternary ammonium group dyeing site that can be dyed on seaweed fibers can be imparted . The five-membered ring quaternary ammonium salt polymer in the embodiment of this application has a structure similar to the M unit of seaweed fibers, has good planarity, is easy to adsorb and cross-link with the M unit, and the probability of replacing Ca is low. The five-membered ring quaternary ammonium salt polymer in the embodiment of this application has a high cation density, so it can also adsorb the polymer chains of various 2+ seaweed fibers, and finally helps the "egg-shell" system to achieve stable dyeing . seaweed fibers, and finally helps the "egg-shell" system to achieve stable dyeing To form a viable seaweed system while simultaneously ensuring the stability and mechanical performance of the seaweed fibers as much as possible. It is possible.
[0034] As described above, the seaweed fibers of the embodiment of this application have good dyeability and are commercially available. Salt-free dyeing can be performed with direct dyes. According to the embodiment of this application, in the spinning process, 5 members Dyeable seaweed fibers produced by adding quaternary amine salt polymers exhibit vivid colors when dyed. It is soft and has excellent durability. During the dyeing process, the fibers can maintain their original shape and show no signs of dissolution. No elephants were generated, and there was no significant decrease in mechanical performance.
[0035] Furthermore, dyeable seaweed fibers, for example, as proposed in the related technology of CN101736440A Compared to fiber manufacturing methods, this related technology involves adding a dendrimer to the spinning raw material. Although a dyed area can be obtained, the problem of the electronegativity of the fiber cannot be solved. In this example, a five-membered ring quaternary amine polymer is added during the spinning and post-processing steps. This solved the problems of stable dyeing locations and electronegativity in dyeable seaweed fibers. In some embodiments of the present invention, the five-membered ring quaternary amine salt polymer is as follows: It is. TIFF0007832614000003.tif4355 (However, R1 is CH3, CH2CH3, CH2(CH2)4CH3, CH2(CH2 ) 10 CH3, CH2(CH2) 16 It is CH3 or C6H5CH2, and R2 is CH 3, CH2CH3, CH2(CH2)4CH3, CH2(CH2) 10 CH3, CH2 ( CH2) 16 It is CH3 or C6H5CH2, and the degree of polymerization n is in the range of 50 to 25000. be.)
[0036] In some embodiments of the present invention, the five-membered ring quaternary amine salt polymer is a water-soluble five-membered ring quaternary amine salt polymer. It is a cyclic quaternary amine salt polymer.
[0037] In some embodiments of the present invention, the content of a five-membered ring quaternary amine salt polymer in seaweed fiber The amount is between 0.1% by mass and 10% by mass.
[0038] In some embodiments of the present invention, the content of a five-membered ring quaternary amine salt polymer in seaweed fiber The amount is between 2% by mass and 8% by mass.
[0039] In some embodiments of the present invention, the content of a five-membered ring quaternary amine salt polymer in seaweed fiber The amount is 4% to 6% by mass. In some embodiments of the present invention, in seaweed fiber The content of the 5-membered ring quaternary amine salt polymer is 5% by mass.
[0040] In some embodiments of the present invention, the five-membered ring quaternary amine salt polymer is a five-membered ring quaternary Mix the amine salt monomer, initiator, and sodium ethylenediaminetetraacetate, and heat at 60°C to 100°C. The product is produced by maintaining the temperature under °C conditions for 1 to 5 hours to obtain a 5-membered ring quaternary amine salt polymer. It will be done. In some embodiments of the present invention, the five-membered ring quaternary amine salt polymer is a five-membered ring quaternary Mix the amine salt monomer, initiator, and sodium ethylenediaminetetraacetate, and heat at 70°C to 90°C. It is produced by maintaining the temperature under these conditions for 2 to 3 hours to obtain a 5-membered ring quaternary amine salt polymer. It can be done. In some embodiments of the present invention, the five-membered ring quaternary amine salt polymer is a five-membered ring quaternary Mix the amine salt monomer, initiator, and sodium ethylenediaminetetraacetate, and heat at 80°C to 85°C. It is produced by maintaining the temperature under these conditions for 2.5 hours to obtain a 5-membered ring quaternary amine salt polymer. ru.
[0041] In the above embodiment, the 5-membered ring quaternary amine salt polymer is controlled by a stirrer, thermometer, and nitrogen gas. It is manufactured using a reactor equipped with an introduction device.
[0042] In the above embodiment, the concentration of the 5-membered ring quaternary amine monomer is 20% to 80%. The initiator concentration is 0.1% to 2%, and sodium ethylenediaminetetraacetate is 0.001% It is approximately 0.01%.
[0043] In the above embodiment, the concentration of the 5-membered ring quaternary amine monomer is 40% to 60%. The initiator concentration is 1% to 1.5%, and the sodium ethylenediaminetetraacetate concentration is 0.004%. It is approximately 0.006%.
[0044] In the above embodiment, the initiator is potassium persulfate, sodium persulfate, ammonium persulfate. Azobisisobutamidine hydrochloride, azodiisobutyronitrile, azobisisohept Contains one or more types of tanitrile.
[0045] In the above embodiments, the five-membered ring quaternary amine salt polymer is specifically a concentration of 20% to 8%. A 0% five-membered ring quaternary amine monomer is subjected to a reaction using a stirrer, thermometer, and nitrogen gas introduction device. In addition to the reagent, next, 0.1% to 2% initiator, and 0.001% to 0.01% ethylenedioxide Sodium tetraacetate was added sequentially, and then nitrogen gas was introduced for 20-40 minutes, followed by 60 The mixture is heated to ~100°C and kept warm for 1 to 5 hours to produce a 5-membered ring quaternary amine salt polymer. It will be manufactured from now on.
[0046] In some embodiments of the present invention, S10 specifically means: Sodium alginate: 5-membered ring quaternary amine salt polymer = 100: (0.001~30) Sodium alginate and a five-membered ring quaternary amine salt polymer are mixed in water in a mass ratio, and then spun. The process includes step S101, which involves obtaining a liquid.
[0047] In some embodiments of the present invention, S10 specifically means: Sodium alginate:5-membered ring quaternary amine salt polymer = 100:(10~20) by mass ratio Sodium alginate and a five-membered ring quaternary amine salt polymer are mixed in water to obtain a spinning solution. This includes step S101.
[0048] In some embodiments of the present invention, S10 specifically means: Sodium alginate: 5-membered ring quaternary amine salt polymer = 100:(12~18) by mass ratio Sodium alginate and a five-membered ring quaternary amine salt polymer are mixed in water to obtain a spinning solution. This includes step S101.
[0049] In some embodiments of the present invention, the concentration of sodium alginate in the spinning solution is 3. It is between % by quantity and 6% by mass.
[0050] In some embodiments of the present invention, the concentration of sodium alginate in the spinning solution is 4. It is between % by quantity and 5% by mass.
[0051] In some embodiments of the present invention, S20 specifically means After the spinning solution obtained in S10 is allowed to stand and degassed, it is extruded into a coagulation bath at a temperature of 40°C to 70°C to coagulate. The process includes step S201, which involves molding to obtain primary fibers.
[0052] In some embodiments of the present invention, S20 specifically means After the spinning solution obtained in S10 is allowed to stand and degassed, it is extruded into a coagulation bath at a temperature of 50°C to 60°C to coagulate. The process includes step S201, which involves molding to obtain primary fibers.
[0053] In some embodiments of the present invention, the coagulation bath has a concentration of 0.01% to 2% by mass. It contains a five-membered ring quaternary amine salt polymer.
[0054] In some embodiments of the present invention, the coagulation bath has a concentration of 0.5% to 1.5% by mass. It contains % of a five-membered ring quaternary amine salt polymer.
[0055] In some embodiments of the present invention, the coagulation bath contains a 5-membered ring quaternary adenomatous phosphate at a concentration of 1% by mass. It contains methyl salt polymers.
[0056] In some embodiments of the present invention, S40 specifically means The seaweed fibers obtained in S30 are immersed in a treatment agent at a temperature of 20-70°C for 5 min to 60 min. The process includes step S401 of immersion treatment.
[0057] In some embodiments of the present invention, S40 specifically means The seaweed fibers obtained in S30 were immersed in a treatment agent at a temperature of 40-50°C for 20 min to 40 m This includes step S401, which involves immersion treatment.
[0058] In some embodiments of the present invention, the treatment agent is the mass of seaweed fibers obtained in S30. It contains 0.5% to 10% of a five-membered ring quaternary amine salt polymer.
[0059] In some embodiments of the present invention, the treatment agent is the mass of seaweed fibers obtained in S30. It contains 2% to 8% of a five-membered ring quaternary amine salt polymer.
[0060] In some embodiments of the present invention, the treatment agent is the mass of seaweed fibers obtained in S30. It contains 4% to 6% of a five-membered ring quaternary amine salt polymer.
[0061] In some embodiments of the present invention, the pH of the coagulation bath in S20 is 4.5 to 6. The answer is 5.
[0062] In some embodiments of the present invention, the pH of the coagulation bath in S20 is 5.
[0063] In some embodiments of the present invention, in S20, the coagulation bath has a concentration of 1% by mass. This is a 6% by mass aqueous solution of calcium chloride.
[0064] In some embodiments of the present invention, in S20, the coagulation bath has a concentration of 2% by mass. This is a 4% by mass aqueous solution of calcium chloride.
[0065] In some embodiments of the present invention, after S40, the manufacturing method is: The step S50 further includes washing and drying the seaweed fibers obtained in S40. Example 1
[0066] (1) Mix 40g of sodium alginate and 1g of a 5-membered ring quaternary amine salt polymer modifier in a solution of 10 Prepared to 00g. (2) Calcium chloride 5% by mass + 5-membered ring quaternary amine salt polymer modifier solution coagulation bath 1% by mass Prepare the solution, adjust the pH of the coagulation bath to 5 with hydrochloric acid, let the spinning solution stand and degas, then dissolve it in the coagulation bath at 40°C. The material was extruded into a liquid, solidified, molded, stretched, and then washed. (3) Dissolve 1 g of a five-membered ring quaternary amine salt polymer modifier in water to prepare 1000 g of immersion solution. Then, the seaweed fibers produced in step (2) are brought into contact with the soaking solution at 30°C and soaked for 20 minutes. After soaking, the material was washed with water and dried to obtain post-processed cross-linked seaweed fibers. Example 2
[0067] (1) 100 g of sodium alginate was dissolved in water to prepare 2000 g of solution. (2) Calcium chloride 6% by mass + 5-membered ring quaternary amine salt polymer modifier solution coagulation bath 1.5% Prepare the % solution, adjust the pH of the coagulation bath to 6 with hydrochloric acid, let the spinning solution stand and degas, then coagulate in a 40°C bath. The material was extruded into an aqueous solution, solidified, molded, stretched, and then washed. (3) Dissolve 6 g of a five-membered ring quaternary amine salt polymer modifier in water to prepare 1000 g of immersion solution. Then, the seaweed fibers produced in step (2) are brought into contact with the soaking solution at 40°C and soaked for 10 minutes. After soaking, the material was washed with water and dried to obtain post-processed cross-linked seaweed fibers. Example 3
[0068] (1) 300 g of sodium alginate was dissolved in water to prepare 4000 g of solution. (2) Prepare a calcium chloride solution coagulation bath of 4.5% by mass, and adjust the pH of the coagulation bath to 5 with hydrochloric acid. Then, after the spinning solution has been allowed to stand and degassed, it is extruded into a coagulation bath aqueous solution and coagulated and molded at 55°C, stretched and washed. Ta. (3) Dissolve 9 g of a 5-membered ring quaternary amine salt polymer modifier in water to prepare 6000 g of immersion solution. Prepare the seaweed fibers produced in step (2) and bring them into contact with the soaking solution at 50°C for 8 minutes. After soaking, the material was washed with water and dried to obtain post-processed cross-linked seaweed fibers. For comparison, the present invention provides an embodiment of a common polyquaternary ammonium salt compound of a non-five-membered ring. Let's use this as an example. Example 4
[0069] (1) Prepare a solution of 1000 g by mixing 40 g of sodium alginate and 1 g of diaminourea polymer. Ta. (2) Prepare a coagulation bath of 5% by mass of calcium chloride + 1% by mass of diaminourea polymer solution, and coagulate The pH of the solid bath is adjusted to 5 with hydrochloric acid, the spinning solution is left to stand and degassed, and then extruded into the solidification bath solution at 40°C. It was then solidified, molded, stretched, and washed. (3) Dissolve 1 g of diaminourea polymer in water to prepare 1000 g of immersion solution, and then step ( 2) The seaweed fibers produced in step 2) are brought into contact with the soaking solution at 30°C and soaked for 20 minutes to complete the soaking process. Afterward, the material was washed with water and dried to obtain post-processed cross-linked seaweed fibers. Figure 1 shows a scanning electron microscope image of a normal seaweed fiber, and Figure 2 shows a scanning electron microscope image of a stainable seaweed fiber. These are electron microscope images. They show ordinary seaweed fibers and stainable seaweed obtained in Examples 1, 2, 3, and 4. Table 1 shows the dyeability of the fibers.
[0070] Table 1 Performance of ordinary seaweed fibers and dyeable seaweed fibers TIFF0007832614000004.tif67154
[0071] The dyeing process for seaweed fibers according to the embodiment of this application is as follows: Direct dyeing with 400g of water. Colors (Direct Scarlet 4BS, Direct Yellow RS, Direct Blue 3RL) Measure out 0.2g and add it, stir to dissolve, add 10g of seaweed fiber at room temperature, 2℃ / mi After raising the temperature to 80°C and staining for 40 minutes, 10 sachets were placed in a 5g / l neutral detergent solution at 90°C. Washed for 1 minute, then cooled, rinsed with water, and dried or air-dried at 80°C.
[0072] Refer to the national standard "GB / T3921-2008 Textile color fastness test, soap wash fastness". The water fastness of the fibers was tested. As a result, the seaweed fibers obtained in Examples 1, 2, 3, and 4 were tested. These are Direct Scarlet 4BS, Direct Yellow RS, and Direct Blue 3RL. The durability against soap washing was level 4 or higher for all of them.
[0073] The terms "first" and "second" in the specification and claims of this application refer to one or more features. Numerical characteristics may be explicitly or implicitly included. Unless otherwise stated in the description of this application. Furthermore, "multiple" means two or more. In addition, "and / or" in the specification and claims " represents at least one of the aforementioned objects, and the character " / " generally This indicates that the related objects before and after it have an "or" relationship.
[0074] In this specification, the terms "one example," "several examples," and "exemplary example" are used interchangeably. Descriptions that refer to "examples," "specific examples," or "several examples" should refer to the embodiments or The specific features, structures, materials, or properties described in relation to the example are at least one of those of the present application. This means that the above terms are included in the embodiments or examples. The expressions do not necessarily refer to the same embodiments or examples. Furthermore, the specific features described may differ. The structure, materials, or properties may be combined in an appropriate manner in any one or more embodiments or examples. They may be combined.
[0075] Although embodiments of the present application are shown and described, these embodiments are based on the principles and objectives of the present application. Various changes, modifications, substitutions and alterations are possible without deviation, and the scope of this application is as stated in the claims. Those skilled in the art will understand that it is limited by and its equivalents.
Claims
[Claim 1] A method for producing seaweed fiber, Sodium alginate: 5-membered ring quaternary amine salt polymer = 100: (0.001-30) The sodium alginate and the five-membered ring quaternary amine salt polymer are mixed in water in a mass ratio. Then, step S10 to obtain the spinning solution, After the spinning solution obtained in S10 is allowed to stand and degassed, the concentration is 0.01% to 2% by mass. The material is extruded into a solidification bath at a temperature of 40°C to 70°C containing a five-membered ring quaternary amine salt polymer and then solidified. Then, step S20 to obtain primary fibers, Step S30 involves stretching and washing the primary fibers obtained in S20 to obtain the seaweed fibers. and, The seaweed fibers obtained in S30 are immersed in a treatment agent at a temperature of 20 to 70°C for 5 min to 60 Step S40 includes a min immersion treatment, The aforementioned treatment agent contains 0.5% to 10% of five-membered material relative to the mass of seaweed fiber obtained in S30. It contains a cyclic quaternary amine salt polymer, The aforementioned five-membered ring quaternary amine salt polymer is shown below: The aforementioned five-membered ring quaternary amine salt polymer is a five-membered ring quaternary amine salt monomer with a concentration of 20% to 80%. This is added to a reactor equipped with a stirrer, thermometer, and nitrogen gas introduction device, and then 0.1% to 2% Add the initiator, 0.001% to 0.01% sodium ethylenediaminetetraacetate sequentially. Afterward, nitrogen gas is introduced for 20-40 minutes, then the temperature is raised to 60-100°C and maintained for 1-5 hours. Manufactured by heating, (However, R 1 is CH 3 , CH 2 CH 3 , CH 2 (CH 2 )< 4 CH 3 , CH 2 (CH 2 It should be noted that there may be some inaccuracies in the original text structure, especially in the part "< 4 ", which seems to have an extra "<". This might need to be confirmed in the original context for a more accurate translation. ) 10 CH 3 ,CH 2 (CH 2 ) 16 CH 3 , or C 6 H 5 CH 2 And R 2 CH 3 CH 2 CH 3 CH 2 (CH) 2 ) 4 CH 3 CH 2 (CH) 2 ) 10 CH 3 CH 2 ( CH 2 ) 16 CH 3 , or C 6 H 5 CH 2 The degree of polymerization n ranges from 50 to 25000. be.) The content of the five-membered ring quaternary amine salt polymer in the seaweed fiber is 0.1% to 10% by mass. And, The concentration of sodium alginate in the spinning solution is 3% by mass to 6% by mass. In S20, the pH of the coagulation bath is 4.5 to 6.5, and / or S2 In step 0, the coagulation bath further comprises an aqueous calcium chloride solution with a concentration of 1% to 6% by mass. Including, After step S40, the seaweed fibers obtained in S40 are subjected to a washing and drying process. S50 also includes, A method for producing seaweed fiber.
Citation Information
Patent Citations
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