Antibacterial and anti-mite intelligent constant temperature fiber and preparation method thereof
By using soy protein modified solution and Chinese herbal plant extract during the fiber preparation process, combined with pre-spinning injection technology, the problems of rough hand feel, serious loss and environmental pollution are solved, and the softness, antibacterial and anti-mites of the fiber are achieved and the softness of the fiber is achieved. Improved temperature regulation durability.
Patent Information
- Application Number
- CN202211558998.8
- Authority / Receiving Office
- CN · China
- Patent Type
- Patents(China)
- Current Assignee / Owner
- Filing Date
- 2022-12-06
- Publication Date
- 2025-02-18
- Estimated Expiration
- 2042-12-06
AI Technical Summary
In the prior art, functional fibers have problems such as rough feel during the preparation process, serious loss of plant extracts and temperature-regulating materials, environmental pollution caused by abuse of acid baths, and poor fiber temperature-regulating and constant temperature performance.
Soy protein modified solution is used to mix with phase change material powder and far-infrared ceramic powder, add ionic dispersant to prepare a temperature-regulating solution, and add Chinese herbal plant extract to the spinning raw liquid to promote the combination of ingredients through pre-spinning injection technology. , reduce loss and reduce the number of acid baths.
The softness and good feel of the fiber are achieved, which significantly reduces the loss rate of plant extracts and temperature-regulating materials, reduces environmental pollution, improves the long-lasting performance of the fiber, and significantly improves the antibacterial and anti-mites effect.
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Abstract
Description
Technical Field
[0001] The invention relates to the field of fiber technology, and in particular to a method for preparing antibacterial and anti-mite intelligent constant temperature fiber. Background Art
[0002] Intelligent temperature-regulating fiber is a high-tech product developed by combining phase change thermal storage material technology with fiber weaving technology. When the external environment temperature rises, textiles containing phase change materials will absorb heat. When the external environment temperature drops, the phase change material releases heat, making the temperature change felt by the human body less obvious, providing a comfortable "microclimate inside the clothes" environment for the human body, so that the human body is always in a comfortable state.
[0003] With the development of society, customers pay more and more attention to the functionality of fibers, especially fibers added with plant extracts, which are the mainstream of functional fibers at present. For example, they have antibacterial, antiviral properties, healthy heating properties, etc. Therefore, combining the functionality of plants with the temperature regulating properties of phase change materials has become the focus of current research.
[0004] The Chinese patent application number is CN202011451740.9, which discloses a rose plant extract cellulose fiber and a preparation method thereof. In order to reduce the loss of plant extracts, a spray circulation bath is added after the conventional spinning bath, which not only increases the difficulty of reusing the coagulation bath, but also causes certain environmental pollution.
[0005] In general, the technology is currently facing the following technical problems: 1. Additive functional fibers feel rough after adding plant extracts and other raw materials; 2. Since the fiber post-processing process has to go through spinning, refining and other processes, the added plant extracts and temperature-regulating materials are lost in great quantities, and the total loss rate even reaches more than 60%, which is a serious waste; 3. Most of them use multiple acid baths to cure to reduce loss, resulting in abuse of acid baths, and cannot be recycled again. Multiple acid baths also cause environmental pollution. 4. Due to the loss of phase change materials, the fiber's long-term temperature regulation and constant temperature performance is poor. Summary of the invention
[0006] In order to make up for the above shortcomings, the present invention provides a method for preparing an antibacterial and anti-mite intelligent constant temperature fiber. The technical problem to be solved by the present invention is:
[0007] 1. Reduce the rough feel of the prepared fiber caused by the addition of temperature regulating materials and plant extracts;
[0008] 2. How to reduce the loss of temperature-regulating materials and plant extracts in the fiber preparation process, improve the reusability of the acid bath, minimize the number of acid baths, and reduce the non-conventional components that do not belong to conventional acid baths.
[0009] 3. Improve the temperature regulation and durability of fibers.
[0010] In order to solve the above technical problems, the technical solution of the present invention is:
[0011] A method for preparing an antibacterial and anti-mite intelligent constant temperature fiber comprises:
[0012] (1) Preparation of soy protein modified solution:
[0013] Grind the soy protein isolate into a particle size of less than 10 μm by an ultrafine powder grinder, add it into deionized water, stir it for 20-30 minutes, add sodium tripolyphosphate, adjust the pH to 8-10, and keep it warm for 30-50 minutes at a certain temperature to obtain a soy protein modified solution;
[0014] Preferably, the amount of sodium tripolyphosphate added is 0.02-0.03% (relative to the amount of soy protein isolate);
[0015] Preferably, the insulation temperature is 40-45°C;
[0016] The mass ratio of the isolated soy protein in the soy protein modified solution is 5-15% (relative to the total mass of the soy protein modified solution);
[0017] The addition of soy protein isolate can make the prepared fiber have a better feel, and at the same time help the fiber to better combine with functional ingredients and reduce loss.
[0018] (2) Preparation of temperature-adjusting solution:
[0019] The phase change material powder, far-infrared ceramic powder and soybean protein modified solution are mixed, an ion dispersant is added during the mixing process, and the mixture is stirred evenly to obtain a temperature regulating solution;
[0020] Preferably, the ionic dispersant is one or more of sodium dodecylbenzene sulfonate, silane coupling agent, and sodium pyrophosphate;
[0021] Preferably, in the temperature-adjusting solution, the mass ratio of the phase change material powder, the far-infrared ceramic powder, and the soy protein modified solution is 1-3:0.2-0.8:10-20;
[0022] Preferably, the phase change material powder is produced by Guangzhou Shengse Technology Co., Ltd., and the average particle size of the phase change material powder is 3±1 μm; the far-infrared ceramic powder is purchased from the market, with a mesh size of 3000-3500.
[0023] (3) Preparation of mixed spinning solution:
[0024] Using 400-550DP cellulose pulp as raw material, through the steps of impregnation, pressing, crushing, aging, yellowing and dissolving, a cellulose spinning solution with 9.0-12.0% cellulose acetone, a viscosity of 65-75s, a maturity of 18-22ml (10% NH4Cl value) and an alkali content of 5.5-7.5% is prepared, and the prepared temperature-adjusting solution is mixed with the cellulose spinning solution in a mixing barrel to obtain a mixed spinning solution;
[0025] Preferably, the amount of the temperature-adjusting solution added to the mixed spinning solution accounts for 5-15 wt % of the total weight of the mixed spinning solution.
[0026] (4) Pre-spinning injection:
[0027] After mixing and filtering three times, the Chinese herbal extract and the mixed spinning solution are mixed in a static mixer through a pre-spinning injection step to prepare a spinning solution; the Chinese herbal plant extract includes an Artemisia argyi extract, a Litsea cubeba extract, tannic acid and a copper sulfate solution;
[0028] Preferably, the amount of the Chinese herbal plant extract added accounts for 1-10% of the mass of the spinning solution.
[0029] Preferably, the mass ratio of the Artemisia argyi extract, the Litsea cubeba extract, the tannic acid aqueous solution and the copper sulfate solution in the Chinese herbal plant extract is 5-10:3-5:30-60:3-15.
[0030] Preferably, the Artemisia argyi extract and Litsea cubeba extract are purchased from the market, and the particle size of the Artemisia argyi extract and Litsea cubeba extract is ≤10 μm;
[0031] Preferably, the preparation and addition method of the Chinese herbal plant extract is as follows: first, a tannic acid aqueous solution with a concentration of 0.5%-2% is prepared, and then the Artemisia argyi extract and the Litsea cubeba extract are added and mixed according to the mass ratio, and the mixed solution is stirred at 10-40°C for 10-20 minutes to mix evenly, and finally, 0.1-0.5 mol / L copper sulfate solution is added before injection, and the spinning stock solution is injected through the pre-spinning injection system to prepare the spinning solution.
[0032] (5) Spinning and post-processing:
[0033] The spinning solution fully mixed with the Chinese herbal medicine plant extract is sent to the spinning machine for spinning, and is ejected from the spinneret through a metering pump, and reacts with the coagulation bath in the acid bath tank, and coagulates and regenerates to form primary fibers;
[0034] Preferably, the concentration of sulfuric acid in the coagulation bath is 140-145 g / L, the concentration of sodium sulfate is 320-350 g / L, and the concentration of zinc sulfate is 15-25 g / L.
[0035] The primary fibers are oriented through drawing and post-treatment processes to form fibers, and then refined and dried to obtain constant temperature intelligent fibers with antibacterial and anti-mite properties; the fibers have a dry breaking strength of 2.1-2.6 cN / dtex, a wet breaking strength of 1.1-1.6 cN / dtex, a melting enthalpy of 44.5-55.6 J / g, and a crystallization enthalpy of 42.4-53.1 J / g; the antibacterial rate against Staphylococcus aureus is more than 98%, the antibacterial rate against Escherichia coli is more than 94%, and the antibacterial rate against Candida albicans is more than 95%. It has a very strong anti-mite effect, with the detection of dust mites being 0 and the avoidance rate being ≥99%.
[0036] Compared with the prior art, the present invention has the following beneficial effects:
[0037] (1) The antibacterial and anti-mite constant temperature intelligent fiber prepared by the present invention has better softness and smooth feel than the same type of temperature regulating functional fiber in the industry due to the addition of soybean protein, and has obvious advantages.
[0038] (2) The present invention successively adds soybean protein and Chinese herbal plant extract solution added by injection before spinning into the spinning solution, wherein the Chinese herbal plant extract solution contains tannic acid and a small amount of copper sulfate. Tannic acid can promote the denaturation and coagulation of the modified soybean protein in the spinning solution, thereby enabling better combination of the phase change material, the plant extract and the cellulose. The addition of soybean protein offsets the roughness of the hand feel caused by the addition of the plant extract and the phase change material, thereby achieving the softness and good hand feel of the fiber. At the same time, the free copper ions in the copper sulfate solution and the two adjacent phenolic hydroxyl groups in the tannic acid can form a stable five-membered ring chelate in the form of oxygen anions, so that the phase change material and the plant extract can be more permanently attached to the fiber, and avoid loss in the subsequent refining, bleaching and other processes. The loss rate of the mugwort extract in the fiber preparation process of the present invention is 3.5-5.0%, and the loss rate of the Litsea cubeba extract is 4.0-6.0%, which are much lower than the loss rate of the functional fiber plant extract in the prior art.
[0039] (3) The present invention achieves the technical effects of good hand feel, fiber functionality and reduced component loss simultaneously by adding a soy protein modified solution to the spinning solution and injecting a Chinese herbal plant extract before spinning, thereby reducing the number of times the coagulation bath is used, avoiding the addition of unnecessary components to the coagulation bath, and reducing environmental pollution.
[0040] (3) The antibacterial and anti-mite intelligent constant temperature fiber and its preparation method can enhance the heat storage and constant temperature function of the fiber by adding a certain mass fraction of temperature regulating material, which is beneficial to ensure the durability and stability of the fiber's thermal insulation. The antibacterial and anti-mite intelligent constant temperature fiber prepared by the present invention is tested using the standard "GB / T 19466.3-2004", with a melting enthalpy of 44.5-55.6 J / g and a crystallization enthalpy of 42.4-53.1 J / g.
[0041] (4) By adding a Chinese herbal plant extract having antibacterial and anti-mite components before the spinning process and modifying the fiber, the antibacterial and anti-mite performance of the fiber can be improved; the antibacterial and anti-mite intelligent constant temperature fiber of the present invention is tested according to the standard of "GB / T20944.3-2008", and the antibacterial rate against Staphylococcus aureus is more than 98%, the antibacterial rate against Escherichia coli is more than 94%, and the antibacterial rate against Candida albicans is more than 95%. The antibacterial and anti-mite intelligent constant temperature fiber of the present invention has a very strong anti-mite effect, with the detection of dust mites being 0 and the avoidance rate being ≥99%. DETAILED DESCRIPTION
[0042] The technical solutions in the embodiments of the present invention are described clearly and completely below. Obviously, the described embodiments are only part of the embodiments of the present invention, not all of them. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without creative work are within the scope of protection of the present invention.
[0043] Example 1
[0044] A preparation method for an antibacterial and anti-mite intelligent constant temperature fiber includes the following preparation steps:
[0045] (1) Preparation of soy protein modified solution:
[0046] The soy protein isolate is ground into a particle size of less than 10 μm by an ultrafine powder grinder, added into deionized water, stirred for 20 minutes, sodium tripolyphosphate is added, the pH is adjusted to 8, and the reaction is kept warm for 50 minutes to obtain a soy protein modified solution; the amount of sodium tripolyphosphate added is 0.03% (relative to the mass of the soy protein isolate); the keeping temperature is 40° C.; the mass ratio of the soy protein isolate in the soy protein modified solution is 10%.
[0047] (2) Preparation of temperature-adjusting solution:
[0048] Phase change material powder, far-infrared ceramic powder and soy protein modified solution are mixed, and an ion dispersant sodium dodecylbenzene sulfonate is added during the mixing process. The mixture is stirred evenly to obtain a temperature regulating solution. In the temperature regulating solution, the mass ratio of phase change material powder, far-infrared ceramic powder and soy protein modified solution is 1:0.3:10. The phase change material powder is produced by Guangzhou Shengse Technology Co., Ltd., and the average particle size of the phase change material powder is 3±1μm. The far-infrared ceramic powder is purchased from the market, 3000 mesh.
[0049] (3) Preparation of mixed spinning solution:
[0050] Using 400DP cellulose pulp as raw material, a cellulose spinning solution with 10.0% acetone, a viscosity of 65s, a maturity of 22ml (10% NH4Cl value) and an alkali content of 5.5% is prepared through the steps of impregnation, pressing, crushing, aging, xanthation and dissolution. The prepared temperature regulating solution is mixed with the cellulose spinning solution in a mixing barrel to obtain a mixed spinning solution; the amount of the temperature regulating solution added to the mixed spinning solution accounts for 5wt% of the total weight of the mixed spinning solution.
[0051] (4) Pre-spinning injection:
[0052] After mixing, the Chinese herbal extract is filtered three times, and the Chinese herbal extract is mixed with the spinning solution in a static mixer through a pre-spinning injection step to prepare a spinning solution; the Chinese herbal plant extract includes mugwort extract, litsea cubeba extract, tannic acid and copper sulfate solution; the amount of the Chinese herbal plant extract added accounts for 5% of the spinning solution mass. The mass ratio of the mugwort extract, litsea cubeba extract, tannic acid solution and copper sulfate solution in the Chinese herbal plant extract is 9:4:50:15, and the particle size of the mugwort extract and litsea cubeba extract is ≤10μm;
[0053] The preparation and addition method of Chinese herbal plant extract is as follows: first, a 2% tannic acid aqueous solution is prepared, and then the Artemisia argyi extract and the Litsea cubeba extract are added and mixed according to the mass ratio. The mixed solution is stirred at 30°C for 10 minutes to mix evenly. Finally, 0.2 mol / L copper sulfate solution is added before injection, and the spinning stock solution is injected through the pre-spinning injection system to prepare the spinning solution.
[0054] (5) Spinning and post-processing:
[0055] The spinning solution fully mixed with Chinese herbal plant extract is sent to the spinning machine for spinning, sprayed out from the spinneret through a metering pump, and reacted with the coagulation bath in the acid bath tank to coagulate and regenerate to form primary fibers; the concentration of sulfuric acid in the coagulation bath is 140g / L, the concentration of sodium sulfate is 320g / L, and the concentration of zinc sulfate is 20g / L.
[0056] The nascent fibers are oriented through drawing and post-treatment processes to form fibers, and then refined and dried to obtain constant temperature intelligent fibers with antibacterial and anti-mite properties; the fibers have a dry breaking strength of 2.4 cN / dtex, a wet breaking strength of 1.3 cN / dtex, a melting enthalpy of 44.7 J / g, and a crystallization enthalpy of 42.4 J / g; the antibacterial rate against Staphylococcus aureus is 98%, the antibacterial rate against Escherichia coli is 94%, and the antibacterial rate against Candida albicans is 95%. The antibacterial and anti-mite intelligent constant temperature fibers of the present invention have a very strong anti-mite effect, with the detection of dust mites being 0 and the avoidance rate being ≥99%.
[0057] Example 2
[0058] The preparation of an antibacterial and anti-mite intelligent constant temperature fiber includes the following preparation steps:
[0059] (1) Preparation of soy protein modified solution:
[0060] The soy protein isolate is ground into a particle size of less than 10 μm by an ultrafine powder grinder, added into deionized water, stirred for 20 minutes, sodium tripolyphosphate is added, the pH is adjusted to 8, and the reaction is kept warm for 50 minutes to obtain a soy protein modified solution; the amount of sodium tripolyphosphate added is 0.03% (relative to the mass of the soy protein isolate); the keeping temperature is 40° C.; the mass ratio of the soy protein isolate in the soy protein modified solution is 10%.
[0061] (2) Preparation of temperature-adjusting solution:
[0062] Phase change material powder, far-infrared ceramic powder and soy protein modified solution are mixed, and an ion dispersant sodium dodecylbenzene sulfonate is added during the mixing process. The mixture is stirred evenly to obtain a temperature regulating solution. In the temperature regulating solution, the mass ratio of phase change material powder, far-infrared ceramic powder and soy protein modified solution is 1:0.3:10. The phase change material powder is produced by Guangzhou Shengse Technology Co., Ltd., and the average particle size of the phase change material powder is 3±1μm. The far-infrared ceramic powder is purchased from the market, 3000 mesh.
[0063] (3) Preparation of mixed spinning solution:
[0064] Using 400DP cellulose pulp as raw material, a cellulose spinning solution with 10.0% acetone, a viscosity of 65s, a maturity of 22ml (10% NH4Cl value) and an alkali content of 5.5% is prepared through the steps of impregnation, pressing, crushing, aging, xanthation and dissolution. The prepared temperature regulating solution is mixed with the cellulose spinning solution in a mixing barrel to obtain a mixed spinning solution; the amount of the temperature regulating solution added to the mixed spinning solution accounts for 10wt% of the total weight of the mixed spinning solution.
[0065] (4) Pre-spinning injection:
[0066] After mixing, the Chinese herbal extract is filtered three times, and the Chinese herbal extract is mixed with the spinning solution in a static mixer through a pre-spinning injection step to prepare a spinning solution; the Chinese herbal plant extract includes mugwort extract, litsea cubeba extract, tannic acid and copper sulfate solution; the amount of the Chinese herbal plant extract added accounts for 5% of the spinning solution mass. The mass ratio of the mugwort extract, litsea cubeba extract, tannic acid solution and copper sulfate solution in the Chinese herbal plant extract is 10:5:50:15, and the particle size of the mugwort extract and litsea cubeba extract is ≤10μm;
[0067] The preparation and addition method of Chinese herbal plant extract is as follows: first, a 2% tannic acid aqueous solution is prepared, and then the Artemisia argyi extract and the Litsea cubeba extract are added and mixed according to the mass ratio. The mixed solution is stirred at 30°C for 10 minutes to mix evenly. Finally, 0.2 mol / L copper sulfate solution is added before injection, and the spinning stock solution is injected through the pre-spinning injection system to prepare the spinning solution.
[0068] (5) Spinning and post-processing:
[0069] The spinning solution fully mixed with Chinese herbal plant extract is sent to the spinning machine for spinning, sprayed out from the spinneret through a metering pump, and reacted with the coagulation bath in the acid bath tank to coagulate and regenerate to form primary fibers; the concentration of sulfuric acid in the coagulation bath is 140g / L, the concentration of sodium sulfate is 320g / L, and the concentration of zinc sulfate is 20g / L.
[0070] The nascent fibers are oriented through drawing and post-treatment processes to form fibers, and then refined and dried to obtain constant temperature intelligent fibers with antibacterial and anti-mite properties; the fibers have a dry breaking strength of 2.1 cN / dtex, a wet breaking strength of 1.1 cN / dtex, a melting enthalpy of 55.6 J / g, and a crystallization enthalpy of 53.1 J / g; the antibacterial rate against Staphylococcus aureus is 99%, the antibacterial rate against Escherichia coli is 98%, and the antibacterial rate against Candida albicans is 99%. The antibacterial and anti-mite intelligent constant temperature fibers of the present invention have a very strong anti-mite effect, with the detection of dust mites being 0 and the avoidance rate being ≥99%.
[0071] Example 3
[0072] The present invention describes the above technical solution in detail through the following embodiments:
[0073] The preparation of an antibacterial and anti-mite intelligent constant temperature fiber includes the following preparation steps:
[0074] (1) Preparation of soy protein modified solution:
[0075] The soy protein isolate is ground into a particle size of less than 10 μm by an ultrafine powder grinder, added into deionized water, stirred for 20 minutes, sodium tripolyphosphate is added, the pH is adjusted to 8, and the reaction is kept warm for 50 minutes to obtain a soy protein modified solution; the amount of sodium tripolyphosphate added is 0.03% (relative to the mass of the soy protein isolate); the keeping temperature is 40° C.; the mass ratio of the soy protein isolate in the soy protein modified solution is 10%.
[0076] (2) Preparation of temperature-adjusting solution:
[0077] Phase change material powder, far-infrared ceramic powder and soy protein modified solution are mixed, and an ion dispersant sodium dodecylbenzene sulfonate is added during the mixing process. The mixture is stirred evenly to obtain a temperature regulating solution. In the temperature regulating solution, the mass ratio of phase change material powder, far-infrared ceramic powder and soy protein modified solution is 1:0.3:10. The phase change material powder is produced by Guangzhou Shengse Technology Co., Ltd., and the average particle size of the phase change material powder is 3±1μm. The far-infrared ceramic powder is purchased from the market, 3000 mesh.
[0078] (3) Preparation of mixed spinning solution:
[0079] Using 400DP cellulose pulp as raw material, a cellulose spinning solution with 10.0% acetone, a viscosity of 65s, a maturity of 22ml (10% NH4Cl value) and an alkali content of 5.5% is prepared through the steps of impregnation, pressing, crushing, aging, xanthation and dissolution. The prepared temperature regulating solution is mixed with the cellulose spinning solution in a mixing barrel to obtain a mixed spinning solution; the amount of the temperature regulating solution added to the mixed spinning solution accounts for 5wt% of the total weight of the mixed spinning solution.
[0080] (4) Pre-spinning injection:
[0081] After mixing, the Chinese herbal extract is filtered three times, and the Chinese herbal extract is mixed with the spinning solution in a static mixer through a pre-spinning injection step to prepare a spinning solution; the Chinese herbal plant extract includes mugwort extract, litsea cubeba extract, tannic acid and copper sulfate solution; the amount of the Chinese herbal plant extract added accounts for 5% of the spinning solution mass. The mass ratio of the mugwort extract, litsea cubeba extract, tannic acid solution and copper sulfate solution in the Chinese herbal plant extract is 8:3:50:15, and the particle size of the mugwort extract and litsea cubeba extract is ≤10μm;
[0082] The preparation and addition method of Chinese herbal plant extract is as follows: first, a 2% tannic acid aqueous solution is prepared, and then the Artemisia argyi extract and the Litsea cubeba extract are added and mixed according to the mass ratio. The mixed solution is stirred at 30°C for 10 minutes to mix evenly. Finally, 0.2 mol / L copper sulfate solution is added before injection, and the spinning stock solution is injected through the pre-spinning injection system to prepare the spinning solution.
[0083] (5) Spinning and post-processing:
[0084] The spinning solution fully mixed with Chinese herbal plant extract is sent to the spinning machine for spinning, sprayed out from the spinneret through a metering pump, and reacted with the coagulation bath in the acid bath tank to coagulate and regenerate to form primary fibers; the concentration of sulfuric acid in the coagulation bath is 140g / L, the concentration of sodium sulfate is 320g / L, and the concentration of zinc sulfate is 20g / L.
[0085] The nascent fibers are oriented through drawing and post-treatment processes to form fibers, and then refined and dried to obtain constant temperature intelligent fibers with antibacterial and anti-mite properties; the fibers have a dry breaking strength of 2.6 cN / dtex, a wet breaking strength of 1.6 cN / dtex, a melting enthalpy of 44.5 J / g, and a crystallization enthalpy of 42.5 J / g; the antibacterial rate against Staphylococcus aureus is 98%, the antibacterial rate against Escherichia coli is 94%, and the antibacterial rate against Candida albicans is 95%. The antibacterial and anti-mite intelligent constant temperature fibers of the present invention have a very strong anti-mite effect, with the detection of dust mites being 0 and the avoidance rate being ≥99%.
[0086] Comparative Example 1
[0087] The present invention describes the above technical solution in detail through the following embodiments:
[0088] The difference between the comparative example and embodiment 1 is:
[0089] On the premise that other process conditions remain unchanged, the added Chinese herbal plant extracts only include Artemisia argyi extract and Litsea cubeba extract, and do not contain tannic acid solution and copper sulfate solution, wherein the mass ratio of Artemisia argyi extract and Litsea cubeba extract is 10:5.
[0090] Comparative Example 2
[0091] The present invention describes the above technical solution in detail through the following embodiments:
[0092] The difference between this comparative example and Example 1 is:
[0093] Under the premise that other process conditions remain unchanged, the amounts of temperature-adjusting solution added to the fiber are 1%, 3%, 16%, 20% and 25% respectively.
[0094] Comparative Example 3
[0095] The present invention describes the above technical solution in detail through the following embodiments:
[0096] The difference between this comparative example and Example 1 is:
[0097] Under the premise that other process conditions remain unchanged, the amount of temperature regulating solution added to the fiber is 0.
[0098] Comparative Example 4
[0099] The present invention describes the above technical solution in detail through the following embodiments:
[0100] The difference between this comparative example and Example 1 is:
[0101] Under the premise that other process conditions remain unchanged, the amount of Chinese herbal plant extract added to the viscose spinning solution through the pre-spinning injection step is 0.
[0102] The difference between Example 1 and Comparative Example 2 and Comparative Example 3 is that: 5% of the temperature-adjusting solution is added in Example 1, while 1%, 3%, 16%, 20% and 25% of the temperature-adjusting solution are added in Comparative Example 2, and no temperature-adjusting solution is added in Comparative Example 3, and other conditions are the same. The specific operation steps are: the fiber is made into a fabric with a thickness of 1 cm, wrapped around the periphery of the temperature recorder probe, placed in a 65°C oven for 35 minutes, taken out and placed at room temperature, and the surface temperature T1 and T2 of the fabric after 20s and 30s are tested to characterize the constant temperature performance of the fiber, as shown in the following table:
[0103]
[0104] As shown in the above table: adding the temperature regulating solution is beneficial to improving the overall heat storage and thermal insulation performance of the fiber, and the cooling rate is significantly slower than that without adding the temperature regulating solution. However, as the mass of the temperature regulating solution added increases, the constant temperature effect tends to be balanced. Therefore, combined with actual production, the preferred addition amount can be 5-15%. In actual production, as the amount of temperature regulating solution added increases, it has a greater impact on the physical properties of the fiber. At the same time, based on cost considerations, the more appropriate addition amount of the temperature regulating solution is 5-15%.
[0105] The difference between Example 1 and Comparative Example 4 is that Chinese herbal plant extract is added in Example 1, while Chinese herbal plant extract is not added in Comparative Example 4. The difference between Example 1 and Comparative Example 1 is that tannic acid and copper sulfate solution are not added in Comparative Example 1.
[0106] In order to prove the excellent antibacterial performance of the antibacterial and anti-mite intelligent constant temperature fiber of the present invention, the antibacterial performance of Examples 1-3 and Comparative Examples 1 and 4 was tested by washing blank cloth 50 times according to the domestic standard GB / T20944.3-2008. The test results are as follows:
[0107]
[0108] It can be seen from the above table that the antibacterial and anti-mite intelligent constant temperature fiber of the present invention has an antibacterial rate of more than 98% against Staphylococcus aureus, an antibacterial rate of more than 94% against Escherichia coli, and an antibacterial rate of more than 95% against Candida albicans.
[0109] As shown in the table above: tannic acid solution and copper sulfate solution are conducive to promoting the mixing of effective ingredients in Chinese herbal plant extracts with fibers, thereby reducing loss and improving the durability of their antibacterial and anti-mite properties. Artemisia argyi is rich in terpenes, flavonoids and aromatic essential oils, which have inhibitory effects on pathogenic bacteria, fungi and viruses, and also have an avoidance effect on mites; Litsea cubeba has high yield and rich resources, among which the main chemical components that have been determined are as high as more than 17 kinds, and their properties and uses are different. The main component citral accounts for more than 80%, which has good antifungal and good antibacterial effects. Tannic acid and copper sulfate solutions can enhance the combination of fibers and effective ingredients in plant extracts. After the content of tannic acid and copper sulfate is reduced, the corresponding antibacterial properties will be slightly reduced. In the case of not adding tannic acid and copper sulfate solutions, the antibacterial properties after multiple washings are significantly reduced. After comparing with the fiber without adding Chinese herbal plant extracts, it can be clearly seen that the antibacterial and anti-mite intelligent constant temperature fiber of the present invention has excellent antibacterial properties.
[0110] Comparative Example 5
[0111] The difference between Comparative Example 5 and Example 1 is that the step of preparing the soy protein modified solution is removed, and the soy protein modified solution is not added in the preparation of the temperature adjustment solution. The various indicators of the prepared antibacterial and anti-mite intelligent constant temperature fiber are as follows (the loss rate is detected by liquid chromatography):
[0112]
[0113] According to the above table, the loss rate of the Artemisia argyi extract in the fiber preparation process of the present invention is 3.5-5.0%, and the loss rate of the Litsea cubeba extract is 4.0-6.0%.
[0114] After removing the preparation step of the soy protein modified solution and not adding the soy protein modified solution in the preparation of the temperature regulating solution, the antibacterial property of the prepared antibacterial and anti-mite intelligent constant temperature fiber was greatly reduced, and the loss rate of the Artemisia argyi extract and the loss rate of the Litsea cubeba extract were greatly increased (≥25%).
[0115] In order to illustrate the excellent anti-mite performance of the antibacterial and anti-mite intelligent constant temperature fiber of the present invention, the anti-mite performance of Example 1 and Comparative Example 4 was tested according to GB / T24253-2009, 9.1 repellency method. The test results are shown in the following table:
[0116] Detection of organisms Dust mites Example 1 0(avoidance rate ≥ 99%) Example 2 0(avoidance rate ≥ 99%) Example 3 0(avoidance rate ≥ 99%) Comparative Example 4 184
[0117] The mite number used in the experiment in the above table is: TT059. It can be seen that the antibacterial and anti-mite intelligent constant temperature fiber of the present invention has an extremely strong anti-mite effect, and the avoidance rate is greater than 99%. The level is: extremely strong anti-mite effect (≥95% is extremely strong; ≥80% is relatively strong; ≥60% is anti-mite effect).
[0118] Secondly, the antibacterial and anti-mite intelligent constant temperature fiber of Example 1 of the present invention was tested for melting temperature, melting enthalpy, crystallization temperature and crystallization enthalpy. The test was carried out in accordance with GB / T 19466.3-2004. The sample was dried at 105° C. for 30 minutes before the test.
[0119] Example Melting enthalpy (J / g) Crystallization enthalpy (J / g) Example 1 44.7 42.4 Example 2 55.6 53.1 Example 3 44.5 42.5
[0120] It can be seen from the above table that the antibacterial and anti-mite intelligent constant temperature fiber prepared by the present invention has a melting enthalpy of 44.5-55.6 J / g and a crystallization enthalpy of 42.4-53.1 J / g.
[0121] It can be seen from the data in the above table that the antibacterial and anti-mite intelligent constant temperature fiber of Example 1 of the present invention has a relatively high melting enthalpy.
[0122] The above shows and describes the basic principles, main features and advantages of the present invention. Those skilled in the art should understand that the present invention is not limited by the above embodiments. The above embodiments and descriptions are only preferred examples of the present invention and are not intended to limit the present invention. Without departing from the spirit and scope of the present invention, the present invention may have various changes and improvements, which fall within the scope of the present invention. The scope of protection of the present invention is defined by the attached claims and their equivalents.
Claims
1. A method for preparing an antibacterial and anti-mite intelligent constant temperature fiber, characterized in that: The fiber preparation method comprises the steps of preparing a soybean protein solution, preparing a temperature-adjusting solution, preparing a mixed spinning solution, pre-spinning injection, spinning and post-treatment. The preparation steps of the soybean protein solution are as follows: grinding the soybean protein isolate by an ultrafine powder grinder to a particle size of less than 10 μm, adding the mixture into deionized water, stirring for 20-30 minutes, adding sodium tripolyphosphate, adjusting the pH value to 8-10, and reacting at a certain temperature for 30-50 minutes; The pre-spinning injection step comprises: mixing the Chinese herbal plant extract with the spinning solution in a static mixer; the Chinese herbal plant extract comprises an artemisia argyi extract, a cassia bark extract, a tannic acid aqueous solution and a copper sulfate solution; and the amount of the Chinese herbal plant extract added accounts for 1-10% of the spinning solution mass.
2. The method for preparing an antibacterial and anti-mite intelligent constant temperature fiber according to claim 1, characterized in that: The amount of sodium tripolyphosphate added is 0.02-0.03% relative to the amount of soy protein isolate.
3. The method for preparing an antibacterial and anti-mite intelligent constant temperature fiber according to claim 1, characterized in that: The insulation temperature is 40-45° C.; the mass ratio of the soy protein isolate in the soy protein solution is 5-15%.
4. The method for preparing the antibacterial and anti-mite intelligent constant temperature fiber according to claim 1, characterized in that: The temperature adjustment solution is prepared by mixing phase change material powder, far infrared ceramic powder and soybean protein solution; In the temperature-adjusting solution, the mass ratio of the phase change material powder, the far-infrared ceramic powder and the soybean protein solution is 1-3:0.2-0.8:10-20.
5. The method for preparing the antibacterial and anti-mite intelligent constant temperature fiber according to claim 4, characterized in that: The average particle size of the phase change material powder is 3±1 μm; the far-infrared ceramic powder is purchased from the market, with a mesh size of 3000-3500.
6. The method for preparing the antibacterial and anti-mite intelligent constant temperature fiber according to claim 1, characterized in that: The amount of the temperature-adjusting solution added to the mixed spinning solution accounts for 5-15 wt % of the total weight of the mixed spinning solution.
7. The method for preparing the antibacterial and anti-mite intelligent constant temperature fiber according to claim 6, characterized in that: The mass ratio of the mugwort extract, the litsea cubeba extract, the tannic acid aqueous solution and the copper sulfate solution in the Chinese herbal plant extract is 5-10:3-5:30-60:3-15.
8. The method for preparing the antibacterial and anti-mite intelligent constant temperature fiber according to claim 7, characterized in that: The mugwort extract and litsea cubeba extract are both purchased from the market, and the particle sizes of the mugwort extract and litsea cubeba extract are ≤10 μm.
9. The method for preparing the antibacterial and anti-mite intelligent constant temperature fiber according to claim 8, characterized in that: The preparation and addition method of the Chinese herbal plant extract is specifically as follows: first, a tannic acid aqueous solution with a concentration of 0.5%-2% is prepared, and then the Artemisia argyi extract and the Litsea cubeba extract are added and mixed according to the mass ratio, and the mixed solution is stirred at 10-40° C. for 10-20 minutes to mix evenly, and finally, a 0.1-0.5 mol / L copper sulfate solution is added before injection, and the spinning solution is injected through the pre-spinning injection system at the same time.
Citation Information
Patent Citations
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