Mosquito-repellent antibacterial cellulose fiber containing wormwood component and preparation method thereof
Technical Field
The invention relates to a mosquito-repellent antibacterial cellulose fiber containing wormwood components and a preparation method thereof, belonging to the technical field of textiles.
Background
In the prior art, various mosquito repelling and killing methods comprise drug killing, smell fumigation, ultraviolet light trapping and the like, mosquito repelling fibers also exist in the market at present, and a yerba mate pompelo clothing company has already provided a mosquito repelling shirt to the market, and the shirt is soaked by citronella essential oil, so that mosquitoes dislike the taste of the citronella essential oil, and therefore, the shirt has a mosquito repelling effect; because the essential oil is volatile, the loss of active ingredients is more in the process of preparing the fiber and using the fiber; in addition, a mosquito repellent insecticide permethrin formula is added into fibers to prepare the mosquito repellent fibers, but the insecticide belongs to chemical components and is not good for health, and the requirements of current consumers on healthy, green and natural products cannot be met.
The natural, herbal and green mosquito repellent components are selected to be added into the fiber independently or compounded with other natural components to prepare the mosquito repellent fiber, and the market prospect is wide.
The isatis root is an excellent traditional Chinese medicinal material and has the effects of resisting bacteria, viruses and tumors and improving the immune function; the isatis root extract is added into viscose fiber to prepare the textile with health care functions of resisting virus, improving immunity and the like, and the textile meets the requirement of the public on products with health care functions at present.
Bluish dogbane, also known as kenaf, tea flower, salix rose, etc., is distributed in northern provinces (autonomous regions) of China Huaihe, Qinling and Kunlun mountains, and has the functions of clearing away fire, lowering blood pressure, strengthening heart, inducing diuresis, treating heart disease, etc.
Wormwood, alias: the plant has strong fragrance, the whole plant is used as a medicine and has the effects of warming channels, removing dampness, dispelling cold, stopping bleeding, diminishing inflammation, relieving asthma, relieving cough, preventing miscarriage, resisting allergy and the like, and the wormwood has a special fragrance which has the effect of repelling mosquitoes.
The functional fiber containing natural and herbaceous plant functional components for repelling mosquitoes, resisting bacteria and resisting viruses in the prior art has the following defects:
(1) the wormwood has a mosquito repellent effect, but when the wormwood is used in the fiber alone, the mosquito repellent effect is general;
(2) in the fiber preparation process, natural and herbal functional components are easy to lose and are easy to be damaged by acid and alkali to cause loss;
(3) functional components on fiber cortex or surface are lost more in the washing and rubbing process, so that the mosquito repellent, antibacterial and antiviral effects of the fiber are reduced.
Disclosure of Invention
Aiming at the defects of the prior art, the invention provides a mosquito-repellent antibacterial cellulose fiber containing wormwood components and a preparation method thereof, so as to realize the following purposes:
(1) the fiber prepared by the invention has good mosquito repellent effect and antifungal and antiviral effects;
(2) in the fiber preparation process, the loss of functional components is reduced;
(3) the fiber prepared by the invention is firmly combined with the fiber by the functional components embedded in the fiber skin layer or the surface in a granular form, and has less loss in the washing and rubbing process.
In order to achieve the purpose of the invention, the invention adopts the technical scheme that:
a mosquito repellent antibacterial cellulose fiber containing folium Artemisiae Argyi component contains chitosan-functional component composite particles 9.0-9.3%, and silicic acid composite colloid 2.2-2.5%.
The following is a further improvement of the above technical solution:
the chitosan-functional component composite particle comprises chitosan, a functional component and starch tertiary amino alkyl ether;
the functional components are a compound of an isatis root extract, an apocynum venetum extract and an artemisia argyi extract; the mass ratio of the isatis root extract to the apocynum venetum extract to the wormwood extract is 1:1: 3; the mass ratio of the sum of the isatis root extract, the apocynum venetum extract and the wormwood extract to the chitosan is 1: 2; the mass ratio of the starch tertiary amino alkyl ether to the chitosan is 1: 3.0-3.3.
A method for preparing mosquito repellent antibacterial cellulose fiber containing folium Artemisiae Argyi component comprises preparing chitosan-functional component composite particles, preparing silicic acid composite colloid, blending, and spinning.
The preparation method of the chitosan-functional component composite particle comprises the steps of dissolving an isatis root extract, an apocynum venetum extract and an artemisia argyi extract in purified water to obtain a functional component solution with the mass concentration of 1.0-1.2 mg/mL; adding the functional component solution into a chitosan acetic acid solution with the mass concentration of 1.4-1.6mg/mL at the speed of 26-30mL/h, controlling the stirring speed to be 350-450r/min, adding starch tertiary amino alkyl ether, uniformly stirring, filtering and defoaming to obtain a chitosan acetic acid solution containing the functional component; then spraying into sodium hydroxide solution at the speed of 5-8ml/min, and granulating to obtain 1-2 micrometer chitosan-functional component composite particles.
The preparation method of the chitosan acetic acid solution comprises the steps of dissolving chitosan in 1% acetic acid solution to obtain 1.4-1.6mg/mL chitosan acetic acid solution, and adjusting the pH value to 4 by 10% acetic acid.
The mass ratio of the isatis root extract to the apocynum venetum extract to the wormwood extract is 1:1: 3;
the mass ratio of the sum of the isatis root extract, the apocynum venetum extract and the wormwood extract to the chitosan is 1: 2;
the mass ratio of the starch tertiary amino alkyl ether to the chitosan is 1: 3.0-3.3.
The preparation of the silicic acid composite colloid comprises the steps of uniformly mixing a 5% sodium silicate aqueous solution with sodium carboxymethylcellulose and starch sulfate, and adding a cross-linking agent N, N-methylene bisacrylamide and a polymerization initiator sodium persulfate to obtain a mixed material; heating the mixed material in a reactor at 45-47 ℃ for 5 hours, adding DL-2000D polyether polyol, slowly heating to 88 ℃ at the speed of 2 ℃/min, controlling the reaction temperature to be 88 +/-2 ℃, introducing nitrogen for pressurization, and controlling the reaction pressure to be below 0.32-0.35MPa for reaction for 2 hours; then adding the mixture into an acid bath to prepare silicic acid composite colloid which is uniformly dispersed in the acid bath.
The mass ratio of the sodium silicate to the sodium carboxymethyl cellulose to the starch sulfate is 4:1: 2;
the mass ratio of the N, N-methylene bisacrylamide to the sodium silicate is as follows: 0.40-0.45: 100;
the mass ratio of the mass of the polymerization initiator sodium persulfate to the mass of the sodium silicate is 0.20-0.24: 100;
the mass ratio of the polyether polyol to the sodium silicate is 1.0-1.2: 100.
The blending is carried out, namely adding the prepared chitosan-functional component composite particles into viscose spinning solution according to a proportion to obtain blended spinning solution;
the mass ratio of the chitosan-functional component composite particles to the alpha cellulose in the viscose stock solution is 0.095-0.097: 1;
the viscose stock solution has the content of alpha cellulose of 8.8-9.0%, the content of total alkali of 2.9-3.1%, the viscosity of 32-35s and the maturity of 14-16ml (10% ammonium chloride value).
The spinning forming, the acid bath contains 5.5-6.0% silicic acid composite colloid, the nozzle drafting: -7 to-3%, inter-disc draft 25 to 27%, three-bath draft 42 to 45%, four-bath draft 16 to 20%, spinning speed 22 to 25m/min, immersion length: 1100-1120 mm, sulfuric acid concentration of 103-107g/l, sodium sulfate 365-370g/l, zinc sulfate of 4-6g/l, acid temperature: and 4, desulfurizing the finished fiber by using sodium sulfite at the temperature of 44.5-45.5 ℃, and performing post-treatment to obtain the finished fiber.
The invention adopts specific nozzle drafting and soaking, so that the filament stays in the acid bath for a long time, the absorption time of chitosan composite ions and silicic acid composite colloid is prolonged, and the loss of functional components is reduced;
the invention adopts the specific chitosan-functional component composite particles and the prepared specific silicic acid composite colloid, and controls the proper concentration of the silicic acid composite colloid in the acid bath, the lower viscosity of the spinning stock solution, the specific acid bath composition and the spinning forming conditions, so that the chitosan-functional component composite particles and the silicic acid composite colloid are just uniformly dispersed on the cortex and the surface of the fiber and are not easy to fall off.
The compound of the isatis root extract, the apocynum venetum extract and the folium artemisiae argyi extract is used as a functional component, the synergistic interaction effect is achieved, and the isatis root extract and the apocynum venetum extract can improve the mosquito repelling effect of the folium artemisiae argyi extract.
Due to the adoption of the technical scheme, the invention achieves the technical effects that:
(1) the mosquito repellent rate of the fiber prepared by the invention reaches 99.5-99.8%; the bacteriostasis rate of the candida albicans is 96.7-97.3%, and the titer of the influenza A virus and the influenza B virus reaches 7-8 by adopting an erythrocyte agglutination method for detection.
(2) The fiber prepared by the invention has the advantages that the content of the chitosan-functional ingredient composite particles is 9.1-9.3%, the content of the silicic acid composite colloid is 2.2-2.5%, and the loss rate of the chitosan-functional ingredient composite particles is 2-4%, so that the loss of the functional extract and the decomposition in strong acid and alkali are reduced.
(3) The functional components of the antibacterial and antiviral fiber prepared by the invention are uniformly distributed on the cortex or the surface of the fiber, so that the mosquito repelling, antiviral and antibacterial effects can be exerted to the greatest extent; the functional components and the fibers are firmly combined, so that the loss of effective substances on the surfaces of the fibers along with water washing or friction can be avoided; tests show that after 50 times of water washing, the loss rate of the chitosan-functional component composite particles is only 0.8-1.2%.
(4) The antibacterial and antiviral fiber prepared by the invention has the dry breaking strength of 2.83-2.86cN/dtex, the wet breaking strength of 1.80-1.82cN/dtex, the elongation at break of 22.9-23.4 percent, good hygroscopicity and the moisture regain of 16.5-17.5 percent.
Detailed Description
The present invention will be described in detail with reference to examples. The following examples will assist those skilled in the art in further understanding the invention, but are not intended to limit the invention in any way. It should be noted that it would be apparent to those skilled in the art that several modifications and improvements can be made without departing from the inventive concept. All falling within the scope of the present invention.
Example 1 preparation method of mosquito repellent antibacterial cellulose fiber containing wormwood component
The method comprises the following steps:
(1) preparation of Chitosan-functional ingredient composite particles
Dissolving radix Isatidis extract, herba Apocyni Veneti extract, and folium Artemisiae Argyi extract in purified water to obtain functional component solution with mass concentration of 1.0 mg/mL; adding the functional component solution into a chitosan acetic acid solution with the mass concentration of 1.4mg/mL at the speed of 26mL/h, controlling the stirring speed to be 350r/min, adding starch tertiary amino alkyl ether, uniformly stirring, filtering and defoaming to obtain a chitosan acetic acid solution containing the functional component; then spraying into sodium hydroxide solution at a speed of 5ml/min, and granulating to obtain 1-2 micrometer chitosan-functional component composite particles.
The preparation method of the chitosan acetic acid solution comprises the steps of dissolving chitosan in 1% acetic acid solution to obtain 1.4mg/mL chitosan acetic acid solution, and adjusting the pH value to 4 by 10% acetic acid.
The mass ratio of the isatis root extract to the apocynum venetum extract to the wormwood extract is 1:1: 3;
the mass ratio of the sum of the isatis root extract, the apocynum venetum extract and the wormwood extract to the chitosan is 1: 2;
the mass ratio of the starch tertiary amino alkyl ether to the chitosan is 1: 3.0.
(2) Preparation of silicic acid composite colloid
Uniformly mixing 5% sodium silicate aqueous solution, sodium carboxymethylcellulose and starch sulfate, and adding a cross-linking agent N, N, -methylene bisacrylamide and a polymerization initiator sodium persulfate to obtain a mixed material; heating the mixed material in a reactor at 45 ℃ for 5 hours, adding DL-2000D polyether polyol, slowly heating to 88 ℃ at the speed of 2 ℃/min, controlling the reaction temperature to be 88 +/-2 ℃, introducing nitrogen for pressurization, and controlling the reaction pressure to be below 0.32MPa for reaction for 2 hours; then adding the mixture into an acid bath to prepare silicic acid composite colloid which is uniformly dispersed in the acid bath.
The mass ratio of the sodium silicate to the sodium carboxymethyl cellulose to the starch sulfate is 4:1: 2;
the mass ratio of the N, N-methylene bisacrylamide to the sodium silicate is as follows: 0.40: 100;
the mass ratio of the mass of the polymerization initiator sodium persulfate to the mass of the sodium silicate is 0.20: 100;
the mass ratio of the polyether polyol to the sodium silicate is 1.0: 100.
(3) Blending of
Adding the prepared chitosan-functional component composite particles into viscose spinning solution according to a proportion to obtain blended spinning solution;
the mass ratio of the chitosan-functional component composite particles to the alpha cellulose in the viscose stock solution is 0.095: 1;
the viscose stock solution has the A cellulose content of 8.8 percent, the total alkali content of 2.9 percent, the viscosity of 32s and the maturity of 14ml (10 percent of ammonium chloride value).
(4) Spinning formation
The spinning forming, the acid bath contains 5.5% silicic acid composite colloid, the nozzle drafting: -7%, inter-disc draw 25%, three bath draw 42%, four bath draw 16%, spinning speed 22m/min, immersion length: 1100 mm, sulfuric acid concentration in the acid bath of 103g/l, sodium sulfate 365g/l, zinc sulfate 4g/l, acid temperature: and 4, desulfurizing the finished fiber by using sodium sulfite at 44.5 ℃, and performing post-treatment to obtain the finished fiber.
The fiber prepared in the embodiment 1 of the invention has the mosquito repellent rate of 99.5 percent; the bacteriostasis rate of the candida albicans is 96.7%, and the titer of the influenza A virus and the influenza B virus reaches 7 by adopting an erythrocyte agglutination method for detection.
In the fiber prepared in the embodiment 1 of the invention, the content of the chitosan-functional component composite particles is 9.1%, the content of the silicic acid composite colloid is 2.2%, and the loss rate of the chitosan-functional component composite particles is 4%, so that the loss of the functional extract and the decomposition in strong acid and alkali are reduced.
The functional components of the fiber prepared in the embodiment 1 of the invention are uniformly distributed on the cortex or the surface of the fiber, so that the mosquito repellent, antiviral and antibacterial effects can be exerted to the greatest extent; the functional components and the fibers are firmly combined, so that the loss of effective substances on the surfaces of the fibers along with water washing or friction can be avoided; tests show that after 50 times of water washing, the loss rate of the chitosan-functional ingredient composite particles is only 0.8%.
The fiber prepared in the embodiment 1 of the invention has the dry breaking strength of 2.83cN/dtex, the wet breaking strength of 1.80cN/dtex, the elongation at break of 22.9 percent, good moisture absorption and the moisture regain of 16.5 percent.
Example 2 preparation method of mosquito repellent antibacterial cellulose fiber containing wormwood component
The method comprises the following steps:
(1) preparation of Chitosan-functional ingredient composite particles
Dissolving radix Isatidis extract, herba Apocyni Veneti extract, and folium Artemisiae Argyi extract in purified water to obtain functional component solution with mass concentration of 1.2 mg/mL; adding the functional component solution into a chitosan acetic acid solution with the mass concentration of 1.6mg/mL at the speed of 30mL/h, controlling the stirring speed to be 450r/min, adding starch tertiary amino alkyl ether, uniformly stirring, filtering and defoaming to obtain a chitosan acetic acid solution containing the functional component; then spraying into sodium hydroxide solution at the speed of 8ml/min, and granulating to obtain 1-2 micrometer chitosan-functional component composite particles.
The preparation method of the chitosan acetic acid solution comprises the steps of dissolving chitosan in 1% acetic acid solution to obtain 1.6mg/mL chitosan acetic acid solution, and adjusting the pH value to 4 by 10% acetic acid.
The mass ratio of the isatis root extract to the apocynum venetum extract to the wormwood extract is 1:1: 3;
the mass ratio of the sum of the isatis root extract, the apocynum venetum extract and the wormwood extract to the chitosan is 1: 2;
the mass ratio of the starch tertiary amino alkyl ether to the chitosan is 1: 3.3.
(2) Preparation of silicic acid composite colloid
Uniformly mixing 5% sodium silicate aqueous solution, sodium carboxymethylcellulose and starch sulfate, and adding a cross-linking agent N, N, -methylene bisacrylamide and a polymerization initiator sodium persulfate to obtain a mixed material; heating the mixed material in a reactor at 47 ℃ for 5 hours, adding DL-2000D polyether polyol, slowly heating to 88 ℃ at the speed of 2 ℃/min, controlling the reaction temperature to be 88 +/-2 ℃, introducing nitrogen for pressurization, and controlling the reaction pressure to be below 0.35MPa for reaction for 2 hours; then adding the mixture into an acid bath to prepare silicic acid composite colloid which is uniformly dispersed in the acid bath.
The mass ratio of the sodium silicate to the sodium carboxymethyl cellulose to the starch sulfate is 4:1: 2;
the mass ratio of the N, N-methylene bisacrylamide to the sodium silicate is as follows: 0.45: 100;
the mass ratio of the mass of the polymerization initiator sodium persulfate to the mass of the sodium silicate is 0.24: 100;
the mass ratio of the polyether polyol to the sodium silicate is 1.2: 100.
(3) Blending of
Adding the prepared chitosan-functional component composite particles into viscose spinning solution according to a proportion to obtain blended spinning solution;
the mass ratio of the chitosan-functional component composite particles to the alpha cellulose in the viscose stock solution is 0.097: 1;
the viscose stock solution contains 9.0% of alpha cellulose, 3.1% of total alkali, 35s of viscosity and 16ml of maturity degree (10% of ammonium chloride value).
(4) Spinning formation
The spinning forming, the acid bath contains 6.0% silicic acid composite colloid, the nozzle drafting: -3%, disc-to-disc draft 27%, three bath draft 45%, four bath draft 20%, spinning speed 25m/min, immersion length: 1120 mm, sulfuric acid concentration in acid bath 107g/l, sodium sulfate 370g/l, zinc sulfate 6g/l, acid temperature: and at 45.5 ℃, desulfurizing the finished fiber by using sodium sulfite, and carrying out post-treatment to obtain a finished fiber product.
The fiber prepared in the embodiment 2 of the invention has the mosquito repellent rate of 99.8 percent; the bacteriostasis rate of the candida albicans is 97.3%, and the titer of the influenza A virus and the influenza B virus reaches 8 by adopting an erythrocyte agglutination method for detection.
In the fiber prepared in the embodiment 2 of the invention, the content of the chitosan-functional component composite particles is 9.3 percent, the content of the silicic acid composite colloid is 2.5 percent, and the loss rate of the chitosan-functional component composite particles is 2 percent, so that the loss of the functional extract and the decomposition in strong acid and alkali are reduced;
the functional components of the fiber prepared in the embodiment 2 of the invention are uniformly distributed on the cortex or the surface of the fiber, so that the mosquito repellent, antiviral and antibacterial effects can be exerted to the greatest extent; the functional components and the fibers are firmly combined, so that the loss of effective substances on the surfaces of the fibers along with water washing or friction can be avoided; tests show that after 50 times of water washing, the loss rate of the chitosan-functional ingredient composite particles is only 1.2%.
The fiber prepared in the embodiment 2 of the invention has the dry breaking strength of 2.86cN/dtex, the wet breaking strength of 1.82cN/dtex, the elongation at break of 23.4 percent, good moisture absorption and the moisture regain of 17.5 percent.
Example 3 synergistic Effect of functional ingredients
On the basis of example 1, only the mass part ratios of the isatis root extract, the apocynum venetum extract and the wormwood extract are changed, the table 1 is changed, and the total amount of the extracts in each test is 5 mass parts; the mosquito repellent effect of the prepared fiber was determined.
TABLE 1 synergistic Effect of functional ingredients
As can be seen from table 1, the combination of the isatis root extract, the apocynum venetum extract and the wormwood extract can improve the mosquito repellent effect of the wormwood extract, and has a synergistic effect.
Unless otherwise stated, the percentages used in the present invention are percentages by weight, and the proportions described in the present invention are proportions by mass.
Finally, it should be noted that: although the present invention has been described in detail with reference to the foregoing embodiments, it will be apparent to those skilled in the art that changes may be made in the embodiments and/or equivalents thereof without departing from the spirit and scope of the invention. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.