Deodorizing fiber, fabric and preparation process thereof
Deodorizing fibers were prepared by loading aminoguanidine salts and sodium alginate/carboxymethyl chitosan onto biomass-based activated carbon, which solved the problems of poor water resistance and low elimination rate of activated carbon-modified deodorizing fibers. This achieved efficient and low-cost deodorization and antibacterial effects, and is suitable for the field of functional fibers.
Patent Information
- Application Number
- CN202411607400.9
- Authority / Receiving Office
- CN · China
- Patent Type
- Patents(China)
- Current Assignee / Owner
- Filing Date
- 2024-11-12
- Publication Date
- 2025-11-18
- Estimated Expiration
- 2044-11-12
AI Technical Summary
In existing technologies, activated carbon-modified deodorizing fibers have poor water washability, low elimination rate of 2-nonenal, high cost, and complex preparation methods.
An odor-deodorizing fiber was prepared by using biomass-based activated carbon loaded with aminoguanidine salt as a deodorizing agent and by using sodium alginate and/or carboxymethyl chitosan as an antibacterial agent and binder through wet spinning technology. The fiber's high porosity and large specific surface area are used to adsorb aldehyde gases, and the antibacterial mechanism of sodium alginate and carboxymethyl chitosan is combined to improve the deodorizing and antibacterial effects.
The prepared deodorizing fiber has excellent water resistance and long-lasting antibacterial and deodorizing properties. The aminoguanidine salt can quickly chemically adsorb aldehyde gas, the by-products are easily volatilized, the antibacterial agent does not affect the softness of the fiber, the cost is low, the process is simple, and it is suitable for industrial applications.
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Abstract
Description
Technical Field
[0001] This application relates to the field of functional fiber technology, and in particular to an odor-eliminating fiber, fabric and its preparation process. Background Technology
[0002] With societal development and an increasingly high proportion of aging population, older adults are prone to accumulating palmitoleic acid (9-hexadecenoic acid) in their sebum. Simultaneously, bacteria on the skin surface ferment and produce palmitoleic acid, which oxidizes and decomposes into 2-nonenal, emitting a candle-like odor. Furthermore, to improve physical fitness, people are increasingly focused on exercise, and sweat after exercise can emit a sour smell. In addition, in social situations, the smell of cigarette smoke clinging to clothing can also cause discomfort.
[0003] As a result, the demand for textiles with deodorizing functions is increasing. Currently, research on textile deodorizing finishing technologies has matured, and deodorizing effects on fabrics can be achieved using chemical or physical methods such as reduction, oxidation, neutralization, addition, condensation, and decomposition.
[0004] Adding activated carbon to fibers can significantly improve their deodorizing performance, especially after modification, giving them a large adsorption capacity and deodorizing function for odors such as ammonia and hydrogen sulfide. However, activated carbon deodorization technology has poor water washability.
[0005] To address the aforementioned issues, existing research, such as the patent publication CN105887227B, discloses a method for preparing antibacterial and deodorizing viscose fibers. This method employs a chemical reduction approach, loading nano-silver ions onto waste wool activated carbon particles, then adding these particles to a viscose spinning solution for wet spinning to obtain the finished antibacterial and deodorizing viscose fibers. The waste wool activated carbon particles are formed by ball milling waste wool activated carbon and have a specific surface area ≥700 m² / g. 2 / g, the activated carbon content in the finished antibacterial and deodorizing viscose fiber is 0.5-4.0%.
[0006] However, the above method using silver ions is relatively expensive. Furthermore, methods that use other chemical antibacterial agents or natural plant antibacterial agents combined with activated carbon for deodorization without adding metal ions have a lower elimination rate for 2-nonenal and are more complex to prepare. Summary of the Invention
[0007] In view of the shortcomings of the prior art, the present invention provides an odor-reducing fiber, fabric and its preparation process to solve the problems of poor water resistance and low elimination rate of 2-nonenal in the prior art.
[0008] To achieve the above and related objectives, the present invention adopts the following technical solution:
[0009] The first aspect of this invention provides a process for preparing deodorizing fibers, comprising the following steps:
[0010] (1) Pre-treat the biomass, mix the pre-treated biomass with an activator, and prepare activated carbon;
[0011] (2) An aminoguanidine salt was loaded onto activated carbon to prepare a deodorant;
[0012] (3) Add the deodorizing agent, antibacterial agent and dispersant to the viscose spinning solution in sequence, mix, and wet spin to obtain deodorizing fiber. The antibacterial agent is sodium alginate and / or carboxymethyl chitosan.
[0013] In one embodiment of this application, step (1) further includes: mixing the pretreated biomass with an activator, activating it under an inert gas atmosphere, cooling it, acid washing it, water washing it, filtering it, and drying it to obtain activated carbon.
[0014] In one embodiment of this application, in step (1), the specific surface area of the activated carbon is 1000-2000 m². 2 / g.
[0015] In one embodiment of this application, in step (1), the biomass is one or more of rice straw, wheat straw, and corn cob;
[0016] And / or, the activator is potassium carbonate and / or potassium hydroxide;
[0017] And / or, the mass ratio of biomass to activator is 1:(1 to 1.5).
[0018] In one embodiment of this application, step (2) further includes: dissolving aminoguanidine salt in water to prepare an impregnation solution, impregnating activated carbon in the impregnation solution to obtain a deodorant, wherein the loading rate of activated carbon is 12-22%.
[0019] In one embodiment of this application, in step (2), the aminoguanidine salt is aminoguanidine sulfate, aminoguanidine nitrate, aminoguanidine carbonate, or aminoguanidine hydrochloride.
[0020] In one embodiment of this application, in step (3), the dispersant is one of sodium silicate, sodium aluminate, ammonium citrate, potassium tripolyphosphate, and potassium pyrophosphate;
[0021] And / or, the mass ratio of deodorant, antibacterial agent, dispersant and viscose spinning solution is (2-5):(0.3-0.8):(0.05-0.1):(94.1-97.65).
[0022] A second aspect of the present invention provides an odor-degrading fiber, which is prepared according to the above-described preparation process.
[0023] A third aspect of the present invention provides an odor-deodorizing fabric, which is woven from the aforementioned odor-deodorizing fibers.
[0024] In one embodiment of this application, the fabric also includes cotton fiber, polyester fiber, silk fiber or wool fiber.
[0025] The beneficial technical effects of this invention are as follows:
[0026] Traditional activated carbon has low porosity and easily reaches adsorption saturation in a short time. Therefore, this invention first prepares biomass-based activated carbon. While reducing costs, the prepared activated carbon has the advantages of high porosity, large specific surface area, and strong adsorption. Using this activated carbon as a porous carrier to load aminoguanidine salts that have deodorizing effects on aldehydes such as 2-nonenal, the elimination rate of odor molecules such as ammonia, acetic acid, and 2-nonenal by the deodorizer can be further improved, and adsorption saturation will not be easily reached.
[0027] This invention utilizes aminoguanidine salts to rapidly and unidirectionally chemically adsorb aldehyde gases at room temperature, undergoing a dehydration reaction to achieve deodorization. Furthermore, the byproducts of the reaction, such as methylene amino compounds, are volatile and can be adsorbed by biomass-based activated carbon, thus posing no negative impact on human health. In addition, existing technologies often add cross-linking agents, such as silane coupling agents and carbamate cross-linking agents, to improve the bonding strength between the deodorizing agent and the fiber in order to address the poor water resistance of deodorizing fibers. However, this approach can negatively impact the fiber's softness and other properties. Moreover, to impart additional functions to the deodorizing fibers, such as antibacterial properties, additional antibacterial agents, such as nano-titanium dioxide, are required, which is costly and involves complex manufacturing processes.
[0028] This invention directly selects sodium alginate and / or carboxymethyl chitosan as both antibacterial agents and binders. Sodium alginate has broad-spectrum antibacterial activity and strong inhibitory effects on various bacteria and fungi. Its antibacterial mechanism mainly includes cell membrane disruption and blocking of microbial nutrient absorption. The antibacterial mechanism of carboxymethyl chitosan includes: 1. By adsorbing onto the cell surface to form a polymer membrane, it blocks the transport of nutrients into the cell, or by adsorbing onto the cell membrane surface, it alters the cell membrane permeability, causing cytoplasmic loss and cell wall separation, thereby playing a bacteriostatic and bactericidal role; 2. Carboxymethyl chitosan penetrates into the cell and adsorbs charged cytoplasm, causing flocculation, disrupting normal cellular physiological activities, or blocking bacterial DNA transcription, thereby inhibiting bacterial reproduction.
[0029] In the preparation process of this invention, since the coagulation bath of wet spinning is a weakly alkaline solution, the carboxyl groups in the antibacterial agent can undergo esterification reaction with the hydroxyl groups in the coagulation bath, thus exhibiting a gel state and having a three-dimensional network structure. Under the action of the dispersant, the deodorizing agent can be carried in this network structure. Moreover, the sodium alginate gel or carboxymethyl chitosan gel has high viscosity, which can fix itself and the deodorizing agent in the fiber matrix, so that the deodorizing fiber has excellent water resistance and long-lasting antibacterial and deodorizing properties, and will not have a negative impact on the softness of the fiber.
[0030] In addition, this invention also controls the specific surface area, loading rate, and dosage of antibacterial agent and dispersant of activated carbon. Firstly, it avoids the self-aggregation and adhesion of deodorizing agent and antibacterial agent, and improves the uniformity of distribution. Secondly, it avoids the antibacterial agent concentration being too high, which would clog the spinneret, and the concentration being too low, which would result in poor antibacterial properties. Thirdly, it ensures that the deodorizing agent has a long-lasting deodorizing effect and avoids reaching adsorption saturation in a short period of time.
[0031] The preparation process of this invention is simple, highly controllable, and low in cost, and has good prospects for industrialization.
[0032] It should be understood that the above general description and the following detailed description are exemplary and explanatory only, and do not limit this application. Detailed Implementation
[0033] Unless otherwise defined, all technical and / or scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention pertains. It should be understood that certain features of the invention (described in the context of separate embodiments for clarity) may also be provided in combination in a single embodiment. Conversely, multiple features of the invention (described in the context of a single embodiment for brevity) may also be provided separately or in any suitable combination or, where appropriate, in any other described embodiment of the invention. Certain features described in the context of various embodiments will not be considered essential features of those embodiments unless the embodiment is inoperable without those elements. The invention is further illustrated below by specific examples; however, it should be noted that the specific process conditions and results described in the embodiments of the invention are merely illustrative and should not be construed as limiting the scope of protection of the invention. All equivalent changes or modifications made in accordance with the spirit and essence of the invention should be covered within the scope of protection of the invention.
[0034] The first aspect of this invention provides a process for preparing deodorizing fibers, comprising the following steps:
[0035] (1) Select at least one of rice straw, wheat straw and corn cob as biomass, wash the biomass multiple times with deionized water, dry it, crush it with a ball mill, and pass it through a 100-150 mesh sieve to obtain pretreated biomass.
[0036] Potassium carbonate and / or potassium hydroxide are selected as activators. Pretreated biomass and activators are mixed at a mass ratio of 1:(1-1.5) and placed in a tube furnace. Under an inert gas atmosphere, the temperature is increased to 600-800℃ at a heating rate of 3-10℃ / min, activated for 100-150min, and then cooled to room temperature at a cooling rate of 1-5℃ / min. The inert gas is nitrogen and / or argon.
[0037] The material is acid-washed with 0.1 mol / L hydrochloric acid or 0.1 mol / L sulfuric acid to remove metallic impurities. Then it is repeatedly washed with deionized water, filtered, and dried to obtain activated carbon.
[0038] In this step, the specific surface area of the activated carbon is 1000–2000 m². 2 / g.
[0039] (2) Dissolve aminoguanidine salt in water to prepare an impregnation solution, and impregnate activated carbon in the impregnation solution to obtain a deodorant, wherein the loading rate of activated carbon is 12-22%.
[0040] In this step, the aminoguanidine salt is aminoguanidine sulfate, aminoguanidine nitrate, aminoguanidine carbonate, or aminoguanidine hydrochloride.
[0041] In this step, parameters such as impregnation solution concentration, impregnation ratio, impregnation temperature, and number of impregnations need to be adjusted according to the load rate, and no specific limits are imposed here.
[0042] (3) Add the deodorizing agent, antibacterial agent and dispersant to the viscose spinning solution in sequence, mix, and wet spin to obtain deodorizing fiber. The antibacterial agent is sodium alginate and / or carboxymethyl chitosan.
[0043] In this step, the dispersant is one of sodium silicate, sodium aluminate, ammonium citrate, potassium tripolyphosphate, and potassium pyrophosphate.
[0044] In this step, the mass ratio of deodorant, antibacterial agent, dispersant and viscose spinning solution is (2-5):(0.3-0.8):(0.05-0.1):(94.1-97.65).
[0045] In this step, wet spinning is the conventional wet spinning spinning process, which will not be described in detail here.
[0046] The present invention also provides an odor-deodorizing fiber, which is prepared according to the above-described preparation process.
[0047] The present invention also provides an odor-deodorizing fabric, which is woven from the above-mentioned odor-deodorizing fibers.
[0048] Furthermore, the fabrics also include cotton fibers, polyester fibers, silk fibers, or wool fibers.
[0049] The present invention will be described in detail below through specific examples and embodiments. It should also be understood that the following embodiments are only for specific illustration of the present invention and should not be construed as limiting the scope of protection of the present invention. Any non-essential improvements and adjustments made by those skilled in the art based on the above description of the present invention are within the scope of protection of the present invention. The specific process parameters, etc., in the following examples are merely examples within a suitable range; that is, those skilled in the art can make appropriate selections within the appropriate range based on the description herein, and are not intended to be limited to the specific values in the examples below.
[0050] Example 1
[0051] (1) The corn cobs were washed with deionized water several times, dried, crushed by ball mill, and passed through a 100-mesh sieve to obtain pretreated corn cobs.
[0052] Potassium hydroxide was selected as the activator. Pretreated corn cobs and potassium hydroxide were mixed at a mass ratio of 1:1 and placed in a tube furnace. Under a nitrogen atmosphere, the temperature was increased to 800℃ at a heating rate of 8℃ / min and activated for 150min. The mixture was then cooled to room temperature at a cooling rate of 3℃ / min.
[0053] The material was acid-washed with 0.1 mol / L hydrochloric acid to remove metallic impurities, then repeatedly washed with deionized water, filtered, and dried to obtain a material with a specific surface area of 1800 m². 2 / g activated carbon.
[0054] (2) Dissolve aminoguanidine hydrochloride in water to prepare an impregnation solution, and impregnate activated carbon in the impregnation solution to obtain a deodorant, wherein the loading rate of activated carbon is 15%.
[0055] (3) The deodorizing agent, sodium alginate, and sodium silicate are added sequentially to the viscose spinning solution, mixed, and wet-spun to obtain deodorizing fibers.
[0056] The mass ratio of deodorant, sodium alginate, sodium silicate, and viscose spinning solution is 3:0.5:0.05:96.45.
[0057] (4) The above-mentioned deodorizing fibers are woven into deodorizing fabric.
[0058] Example 2
[0059] (1) The corn cobs were washed with deionized water multiple times, dried, crushed using a ball mill, and passed through a 120-mesh sieve to obtain pretreated corn cobs.
[0060] Potassium hydroxide was selected as the activator. Pretreated corn cobs and potassium hydroxide were mixed at a mass ratio of 1:1.2 and placed in a tube furnace. Under a nitrogen atmosphere, the temperature was increased to 800℃ at a heating rate of 8℃ / min and activated for 150min. The mixture was then cooled to room temperature at a cooling rate of 3℃ / min.
[0061] The material was acid-washed with 0.1 mol / L hydrochloric acid to remove metallic impurities, then repeatedly washed with deionized water, filtered, and dried to obtain a material with a specific surface area of 1900 m². 2 / g activated carbon.
[0062] (2) Dissolve aminoguanidine hydrochloride in water to prepare an impregnation solution, and impregnate activated carbon in the impregnation solution to obtain a deodorant, wherein the loading rate of activated carbon is 18%.
[0063] (3) The deodorizing agent, sodium alginate, and sodium silicate are added sequentially to the viscose spinning solution, mixed, and wet-spun to obtain deodorizing fibers.
[0064] The mass ratio of deodorant, sodium alginate, sodium silicate and viscose spinning solution is 5:0.5:0.1:94.4.
[0065] (4) The above-mentioned deodorizing fibers are woven into deodorizing fabric.
[0066] Example 3
[0067] (1) The wheat straw was washed multiple times with deionized water, dried, crushed using a ball mill, and passed through a 150-mesh sieve to obtain pretreated wheat straw.
[0068] Potassium hydroxide was selected as the activator. Pretreated wheat straw and potassium hydroxide were mixed at a mass ratio of 1:1.5 and placed in a tube furnace. Under a nitrogen atmosphere, the temperature was increased to 800℃ at a heating rate of 8℃ / min and activated for 150min. The mixture was then cooled to room temperature at a cooling rate of 3℃ / min.
[0069] The material was acid-washed with 0.1 mol / L hydrochloric acid to remove metallic impurities, then repeatedly washed with deionized water, filtered, and dried to obtain a material with a specific surface area of 1800 m². 2 / g activated carbon.
[0070] (2) Dissolve aminoguanidine sulfate in water to prepare an impregnation solution, and impregnate activated carbon in the impregnation solution to obtain a deodorant, wherein the loading rate of activated carbon is 20%.
[0071] (3) The deodorizing agent, carboxymethyl chitosan, and sodium silicate are added sequentially to the viscose spinning solution, mixed, and wet-spun to obtain deodorizing fibers.
[0072] The mass ratio of deodorant, carboxymethyl chitosan, sodium silicate and viscose spinning solution is 5:0.8:0.1:94.1.
[0073] (4) The above-mentioned deodorizing fibers are woven into deodorizing fabric.
[0074] Example 4
[0075] (1) The rice straw was washed multiple times with deionized water, dried, crushed using a ball mill, and passed through a 150-mesh sieve to obtain pretreated rice straw.
[0076] Potassium hydroxide was selected as the activator. Pretreated rice straw and potassium hydroxide were mixed at a mass ratio of 1:1.5 and placed in a tube furnace. Under a nitrogen atmosphere, the temperature was increased to 800℃ at a heating rate of 8℃ / min and activated for 150min. The mixture was then cooled to room temperature at a cooling rate of 3℃ / min.
[0077] The material was acid-washed with 0.1 mol / L hydrochloric acid to remove metallic impurities, then repeatedly washed with deionized water, filtered, and dried to obtain a material with a specific surface area of 1800 m². 2 / g activated carbon.
[0078] (2) Dissolve aminoguanidine hydrochloride in water to prepare an impregnation solution, and impregnate activated carbon in the impregnation solution to obtain a deodorant, wherein the loading rate of activated carbon is 22%.
[0079] (3) The deodorizing agent, sodium alginate, and sodium silicate are added sequentially to the viscose spinning solution, mixed, and wet-spun to obtain deodorizing fibers.
[0080] The mass ratio of deodorant, sodium alginate, sodium silicate and viscose spinning solution is 5:0.3:0.05:94.65.
[0081] (4) The above-mentioned deodorizing fibers are woven into deodorizing fabric.
[0082] Comparative Example 1
[0083] The difference between this comparative example and Example 1 is as follows:
[0084] The activated carbon is commercially available wood-based activated carbon with a specific surface area of 700 m². 2 / g.
[0085] Comparative Example 2
[0086] The difference between this comparative example and Example 1 is as follows:
[0087] The activated carbon prepared in step (1) was used as a deodorizing agent.
[0088] Comparative Example 3
[0089] The difference between this comparative example and Example 1 is as follows:
[0090] The activated carbon loading rate is 30%.
[0091] Comparative Example 4
[0092] The difference between this comparative example and Example 1 is as follows:
[0093] The deodorizing agent and sodium silicate were added to the viscose spinning solution in sequence, mixed, and wet-spun to obtain deodorizing fiber. The mass ratio of the deodorizing agent, sodium silicate and viscose spinning solution was 3:0.05:96.95.
[0094] Comparative Example 5
[0095] The difference between this comparative example and Example 1 is as follows:
[0096] Deodorizing agent, sodium alginate, and sodium silicate were added sequentially to the viscose spinning solution, mixed, and then wet-spun to obtain deodorizing fibers.
[0097] The mass ratio of deodorant, sodium alginate, sodium silicate, and viscose spinning solution is 5:3:0.05:91.95.
[0098] Performance testing
[0099] Antibacterial properties: The antibacterial properties of the fabric before and after treatment against Staphylococcus aureus ATCC6538, Escherichia coli ATCC25922 and Candida albicans ATCC10231 were determined by shaking flask method according to GB / T 20944.3-2008 "Evaluation of antibacterial properties of textiles - Part 3: Shaking method".
[0100] Antimicrobial properties were tested on the deodorizing fabrics of Examples 1-4 and the fabrics of Comparative Examples 1-5, and the results were recorded as the initial antimicrobial rate. Then, the deodorizing fabrics prepared in the examples and the fabrics prepared in the comparative examples were washed as follows: At 25°C, the deodorizing fabrics prepared in the examples and the fabrics prepared in the comparative examples were immersed in a 20% sodium stearate solution for 5 minutes, then rinsed 5 times with clean water, and dried to complete one washing cycle. The deodorizing fabrics prepared in the examples and the fabrics prepared in the comparative examples were washed 10 times and 20 times, respectively. The antimicrobial test results are shown in Tables 1 and 2.
[0101] Dissolution of antibacterial substances: The dissolution of antibacterial substances was tested according to Appendix A of GB / T 31713-2015, specifically as follows:
[0102] Examples 1-4 were woven with deodorizing fabric with specifications of 40s*40s / 144*85, and three 1.5cm*1.5cm fabric samples were cut from different parts of the fabric in each example as test samples.
[0103] Comparative examples 1 to 5 were woven with fabrics of specifications of 40s*40s / 144*85, and three 1.5cm*1.5cm fabric samples were cut from different parts of each comparative example fabric as test samples.
[0104] Three pieces of two-layer 100% polyester knitted fabric sewn together were used as wash diapers. The mass per unit area of each piece of fabric was 125% of the mass per unit area of the sample to be tested. Each piece of wash diapers was 30cm*30cm in size.
[0105] Each of the above-mentioned test samples, test specimens, and accompanying fabrics should be washed once according to the requirements of Appendix B and Appendix C of FZ / T 73023-2006, and then set aside for use.
[0106] Prepare several standard blank samples according to Appendix A of FZ / T 73023-2006, cut them to 1.5cm*1.5cm, wash them once according to Appendix B of FZ / T 73023-2006, and set them aside for use;
[0107] After washing, sterilize the standard blank samples, each test sample, and each test sample at 103 kPa and 121 °C for 15 min for later use.
[0108] Staphylococcus aureus (ATCC 6538), Escherichia coli (ATCC 25922), and Candida albicans (ATCC 10231) were selected as test strains. Multiple sets of antimicrobial dissolution tests were conducted on the sterilized standard blank, each test sample, and each sample to be tested. The dissolution of antimicrobial substances in each test sample and sample was determined based on the maximum inhibition zone width (D) against Staphylococcus aureus, Escherichia coli, and Candida albicans. The test results are shown in Table 3.
[0109] Odor deodorization performance of textiles: The odor deodorization performance of the deodorizing fabrics prepared in Examples 1-4 and the fabrics prepared in Comparative Examples 1-5 were tested according to GB / T 33610.3-2019 "Determination of odor deodorization performance of textiles", as follows:
[0110] The reagents include: ammonia, acetic acid sample gas, isovaleric acid (purity 98.0%), 2-nonenal (purity 95.0%), dilution gas (nitrogen with purity of 99.99% or higher), and ethanol (analytical grade).
[0111] Take the dimension as (50±2.5)cm 2Four pieces each of the deodorizing fabrics in Examples 1-4 and Comparative Examples 1-4 were used as test samples.
[0112] Gas chromatography: Prepare several 500mL glass conical flasks, half of which are used for sample testing and the other half for blank detection. The fabrics of each example and comparative example are tested separately for isovaleric acid and 2-nonenal.
[0113] Before testing, purge the conical flask with nitrogen gas at a volume greater than 5 times that of the flask, and adjust the humidity and test environment.
[0114] Accurately weigh 20g of isovaleric acid into a volumetric flask and dilute to the mark with ethanol; accurately weigh 10g of 2-nonenal into a volumetric flask and dilute to the mark with ethanol.
[0115] Each of the above-mentioned test samples was used for isovaleric acid and 2-nonenal testing, respectively. Each test sample was laid flat at the bottom of an Erlenmeyer flask, and 1000 mL of nitrogen gas was blown into the flask to expel the air inside. The flask opening was then sealed with a sealing film. Using a syringe, 5 μL of the prepared isovaleric acid and 2-nonenal solution was injected through the sealing film along the inner wall of the Erlenmeyer flask, ensuring that the solution did not come into contact with the test samples. The needle hole was then sealed again with a sealing film.
[0116] Let it stand for 2 hours under the standard atmospheric conditions specified in GB / T 6529.
[0117] For blank testing, repeat the above steps without placing the test sample.
[0118] After 2 hours of contact, hold the conical flask by the mouth and shake it vigorously about 20 times within 20 seconds, with or without the test sample. Insert the gas-tight injection needle vertically about 4 cm into the center of the sealing membrane at the mouth of the conical flask. Use the gas-tight injection needle to draw the test gas from the flask; the sample volume depends on the type of gas chromatograph used.
[0119] Detection tube method: Place each sample to be tested in a sampling bag, evacuate the gas in the sampling bag using a vacuum pump or vacuum pump, inject 3L of ammonia and acetic acid sample gas into the sampling bag respectively using an air pump, let stand for 2 hours, and use a 100mL syringe to extract 100mL of the gas to be tested from each sampling bag containing the sample, and read the color change position scale through the detection tube.
[0120] The ORR% (Organic Rate of Reduction) of odor chemical components was calculated, and the results are shown in Table 4.
[0121] Adsorption saturation: Take the deodorant fabric of Example 1, the fabrics of Comparative Examples 1, 3, and 5 as the test samples. Cut each test sample into a size of 25 cm × 25 cm, and place them in a test chamber filled with odor gas respectively. Use a gas detector at regular intervals to detect the change in the concentration of odor gas in the test chamber. When the concentration no longer changes, the test sample reaches adsorption saturation, record the time when the concentration no longer changes, and the test results are shown in Table 5.
[0122] The experimental data and analysis are as follows:
[0123] Table 1 Antibacterial test results of fabrics in each example and each comparative example 1
[0124]
[0125] Table 2 Antibacterial test results of fabrics in each example and each comparative example 2
[0126]
[0127]
[0128] (Note: The antibacterial rate against Staphylococcus aureus and Escherichia coli ≥ 70%, the antibacterial rate against Candida albicans ≥ 60%, and the sample has antibacterial effect)
[0129] As can be seen from Table 1 and Table 2, after adding antibacterial agents to the viscose spinning dope, the wash resistance of the deodorant fabric is significantly improved, and it has long-term antibacterial performance. After 20 washes, the antibacterial rate drops between 4% and 7%. When no antibacterial agent is added, such as in Comparative Example 4, its antibacterial rate drops by about 25%, its wash resistance is poor, and it does not have antibacterial property after multiple washes.
[0130] In addition, from the data of Examples 1 - 4 and Comparative Examples 1 - 2, it can be seen that the biomass-based activated carbon of the present invention has better antibacterial effect compared with conventional activated carbon and activated carbon with small specific surface area.
[0131] The antibacterial rate of the examples of the present invention is close to that of Comparative Examples 3 and 5, but the dosage in the examples is lower. Considering from the perspective of cost, the parameters of the examples of the present invention are preferred.
[0132] Table 3 Antibacterial substance dissolution test of fabrics in each example and Comparative Examples 1 - 3
[0133]
[0134]
[0135] (Note: The width of the antibacterial zone D: D ≤ 1 mm is non-dissolving, 1 mm < D ≤ 5 mm is slightly dissolving, 5 mm < D ≤ 10 mm is moderately dissolving, D > 10 mm is dissolving)
[0136] Table 3 shows that after adding antibacterial agents to the viscose spinning solution, both the deodorizing agent and the antibacterial agent showed good adhesion to the fibers. The maximum antibacterial zone width of the deodorizing fabric was <1.5mm, and the antibacterial substances exhibited both non-dissolution and good slight dissolution properties. This indicates that the deodorizing fabric with added antibacterial agents will not harm human health and is safer and more reliable. In contrast, the fabric in Comparative Example 4 showed moderate dissolution of antibacterial substances, and its safety was lower than that of the antibacterial and deodorizing fabric of this invention.
[0137] Table 4. Odor deodorization performance of fabrics in each embodiment and comparative example.
[0138] Test object Ammonia ORR / % Acetic acid ORR / % Isovalerate ORR / % 2-Nonenal ORR / % Example 1 87.7 87.0 88.1 90.8 Example 2 90.7 91.4 91.8 92.9 Example 3 91.4 92.6 92.1 93.7 Example 4 91.6 91.5 93.6 93.0 Comparative Example 1 81.7 82.0 80.6 85.7 Comparative Example 2 83.3 85.1 84.9 75.0 Comparative Example 3 91.0 90.8 92.5 93.4 Comparative Example 4 82.2 81.6 80.1 83.6 Comparative Example 5 92.0 91.4 92.5 93.3
[0139] As shown in Table 4, the combination of biomass-based activated carbon with aminoguanidine hydrochloride and antibacterial agents can improve the deodorizing performance of deodorizing fabrics, significantly increase the reduction rate of 2-nonenal, and have strong adsorption capacity for odor molecules.
[0140] Comparative Example 1 shows that the activated carbon has a smaller specific surface area and its adsorption capacity is not as good as the deodorizing fabric of the present invention.
[0141] Comparative Example 2: The activated carbon has a small specific surface area and does not contain aminoguanidine salts, resulting in poor adsorption of 2-nonenal and poor deodorization.
[0142] The sodium alginate and carboxymethyl chitosan used in this invention also have certain deodorizing effects and can work synergistically with activated carbon. Therefore, Comparative Example 4, which does not contain antibacterial agents, has a less effective deodorizing effect than the deodorizing fabric in the embodiments of this invention.
[0143] Table 5. Adsorption saturation test of fabrics in the examples and comparative examples.
[0144] Test object Total time to reach adsorption saturation / h Example 1 56 Comparative Example 1 23 Comparative Example 3 30 Comparative Example 5 26
[0145] As shown in Table 5, the deodorizing fabric prepared in the embodiments of the present invention has a long-lasting deodorizing effect, a long adsorption time, high adsorption capacity, and is not easy to reach adsorption saturation.
[0146] In contrast, the activated carbon in Comparative Example 1 has a small specific surface area and poor adsorption capacity, making it easy to reach adsorption saturation.
[0147] The high loading rate of activated carbon in Comparative Example 3 affects the porosity of activated carbon to a certain extent, reducing its total adsorption capacity and thus making it easier to reach adsorption saturation.
[0148] In Comparative Example 5, the sodium alginate content was too high. On the one hand, it was easy to clog the spinneret during the spinning process, and on the other hand, it reduced the porosity of the activated carbon, affecting its adsorption capacity and thus making it easy to reach adsorption saturation.
[0149] The above embodiments are merely illustrative of the principles and effects of the present invention and are not intended to limit the invention. Any person skilled in the art can modify or alter the above embodiments without departing from the spirit and scope of the present invention. Therefore, all equivalent modifications or alterations made by those skilled in the art without departing from the spirit and technical concept disclosed in the present invention should still be covered by the claims of the present invention.
Claims
1. A process for preparing deodorizing fibers, characterized in that, Includes the following steps: (1) Pre-treat the biomass, mix the pre-treated biomass with an activator to prepare activated carbon, wherein the specific surface area of the activated carbon is 1000~2000 m². 2 / g; (2) An aminoguanidine salt is loaded onto the activated carbon to prepare a deodorant; (3) The deodorizing agent, antibacterial agent and dispersant are added to the viscose spinning solution in sequence, mixed and wet-spun to obtain the deodorizing fiber, wherein the antibacterial agent is sodium alginate and / or carboxymethyl chitosan, and the dispersant is one of sodium silicate, sodium aluminate, ammonium citrate, potassium tripolyphosphate or potassium pyrophosphate.
2. The preparation process according to claim 1, characterized in that, Step (1) further includes: mixing the pretreated biomass with an activator, activating, cooling, acid washing, water washing, filtering, and drying under an inert gas atmosphere to obtain the activated carbon.
3. The preparation process according to claim 1, characterized in that, In step (1), the biomass is one or more of rice straw, wheat straw, and corn cob; And / or, the activator is potassium carbonate and / or potassium hydroxide; And / or, the mass ratio of the biomass to the activator is 1:(1~1.5).
4. The preparation process according to claim 1, characterized in that, Step (2) further includes: dissolving the aminoguanidine salt in water to prepare an impregnation solution, impregnating the activated carbon in the impregnation solution to obtain the deodorizer, wherein the loading rate of the activated carbon is 12~22%.
5. The preparation process according to claim 1, characterized in that, In step (2), the aminoguanidine salt is aminoguanidine sulfate, aminoguanidine nitrate, aminoguanidine carbonate, or aminoguanidine hydrochloride.
6. The preparation process according to claim 1, characterized in that, The mass ratio of deodorant, antibacterial agent, dispersant and viscose spinning solution is (2~5): (0.3~0.8): (0.05~0.1): (94.1~97.65).
7. An odor-deodorizing fiber, characterized in that, The fiber is prepared by the process according to any one of claims 1 to 6.
8. An odor-deodorizing fabric, characterized in that, The fabric is woven from the deodorizing fiber described in claim 7.
9. The deodorizing fabric according to claim 8, characterized in that, The fabric also includes cotton fiber, polyester fiber, silk fiber or wool fiber.
Citation Information
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