CN116988198A - A kind of preparation method of anti-mite mosaic spinning yarn - Google Patents
A kind of preparation method of anti-mite mosaic spinning yarn Download PDFInfo
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- CN116988198A CN116988198A CN202310831027.4A CN202310831027A CN116988198A CN 116988198 A CN116988198 A CN 116988198A CN 202310831027 A CN202310831027 A CN 202310831027A CN 116988198 A CN116988198 A CN 116988198A
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F1/00—General methods for the manufacture of artificial filaments or the like
- D01F1/02—Addition of substances to the spinning solution or to the melt
- D01F1/10—Other agents for modifying properties
- D01F1/103—Agents inhibiting growth of microorganisms
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F6/00—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof
- D01F6/44—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from mixtures of polymers obtained by reactions only involving carbon-to-carbon unsaturated bonds as major constituent with other polymers or low-molecular-weight compounds
- D01F6/54—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from mixtures of polymers obtained by reactions only involving carbon-to-carbon unsaturated bonds as major constituent with other polymers or low-molecular-weight compounds of polymers of unsaturated nitriles
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- D—TEXTILES; PAPER
- D02—YARNS; MECHANICAL FINISHING OF YARNS OR ROPES; WARPING OR BEAMING
- D02G—CRIMPING OR CURLING FIBRES, FILAMENTS, THREADS, OR YARNS; YARNS OR THREADS
- D02G3/00—Yarns or threads, e.g. fancy yarns; Processes or apparatus for the production thereof, not otherwise provided for
- D02G3/22—Yarns or threads characterised by constructional features, e.g. blending, filament/fibre
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- D—TEXTILES; PAPER
- D02—YARNS; MECHANICAL FINISHING OF YARNS OR ROPES; WARPING OR BEAMING
- D02G—CRIMPING OR CURLING FIBRES, FILAMENTS, THREADS, OR YARNS; YARNS OR THREADS
- D02G3/00—Yarns or threads, e.g. fancy yarns; Processes or apparatus for the production thereof, not otherwise provided for
- D02G3/44—Yarns or threads characterised by the purpose for which they are designed
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- Chemical Or Physical Treatment Of Fibers (AREA)
Abstract
本发明涉及一种防螨镶嵌纺纱线的制备方法，传统微胶囊的粒径为微米级别，亚微米纤维难以将其完全包覆，通过调整各种工艺参数，实现对微胶囊粒径的有效控制，制备一种粒径为纳米尺度200～700nm的防螨微胶囊，通过静电成型技术得到包裹防螨微胶囊的亚微米纤维，防止防螨微胶囊脱落。随后将其用于镶嵌纺当中与棉纤维复合。本发明制备防螨微胶囊并对粒径进行了调控，使其适于镶嵌纺，得到舒适耐用的防螨效果持久的棉纱。
The invention relates to a method for preparing anti-mite inlaid spinning yarn. The particle size of traditional microcapsules is at the micron level, and it is difficult to completely cover it with sub-micron fibers. By adjusting various process parameters, the effective control of the particle size of the microcapsules is achieved. Control, prepare an anti-mite microcapsule with a particle size of 200 to 700 nm at the nanoscale, and use electrostatic molding technology to obtain sub-micron fibers wrapping the anti-mite microcapsules to prevent the anti-mite microcapsules from falling off. It is then used in inlay spinning to combine with cotton fibers. The present invention prepares anti-mite microcapsules and regulates the particle size, making it suitable for mosaic spinning, and obtains comfortable and durable cotton yarn with long-lasting anti-mite effect.
Description
Technical Field
The application belongs to the field of textile manufacturing, and particularly relates to a preparation method of anti-mite inlaid spun yarns.
Background
Mite secretions, faeces and mite carcasses are one of the most prominent allergens responsible for allergic diseases, and among all kinds, the most abundant, widespread type of mites are dust mites. Dust mites are suitable for survival under warm and humid environment conditions, and carcasses, faeces and other excretions generated by the dust mites are harmful to human skin health and are easy to cause diseases such as asthma, allergic rhinitis, dermatitis and the like. In the household environment, household textiles such as furniture soft packages, bedclothes and the like are loose and porous, and human body dander remains, so that a proper survival condition is provided for dust mites, and the household textiles are main pathogenic mediums of dust mite transmission diseases, and therefore the development significance of the anti-mite household textiles is great.
The microcapsules can store functional substances, and the anti-mite agent can be stored inside the microcapsules and released when necessary. The existing anti-mite textiles mostly adopt a mode of dipping or spraying finishing agent to enable microcapsules to be attached to cotton yarns or cotton fabrics, the microcapsules are easy to fall off or break, the anti-mite agent is suddenly released, and durable effect cannot be achieved. The development of the inlaid textile anti-mite composite yarn can not only effectively prevent mites from breeding on the surfaces of skin-adhering household textiles and reduce the quantity of allergens related to the skin-adhering household textiles, but also keep the comfort of cotton fabrics and improve the use experience of people. But the particle size of the anti-mite auxiliary agent required by the mosaic spinning is smaller, the particle size of the traditional microcapsule is in the micron level, and the particle size of the microcapsule prepared by the traditional method is not matched with the fineness of the fiber.
Patent CN103147409B discloses an antibacterial and anti-mite microcapsule and a preparation method thereof, wherein polymethyl methacrylate added with silver ions is used as a wall material, and an antibacterial and anti-mite liquid is used as a core material to prepare the antibacterial and anti-mite microcapsule, so that the process is complex and the cost is high.
Patent CN110205827B discloses a manufacturing method of natural antibiotic anti-mite deodorizing Korean pine microcapsule mattress, the antibiotic anti-mite mattress is obtained by spraying microcapsule finishing agent, but the washing resistance is poor, and the comfortableness when in use can be affected when the functional finishing agent is sprayed on the surface of fabric.
Patent CN111270327a discloses a functional fiber for preventing mosquitoes and mites and a preparation method thereof, the fiber for preventing mosquitoes and mites is prepared by preparing microcapsules and blending and spinning with other components, wherein the average particle size of the microcapsules is 10 μm, and after blending spinning is finished, part of the microcapsules are exposed on the surface of the fiber, so that the durability is affected.
Disclosure of Invention
Aiming at the defects of the prior art, the technical problem to be solved by the application is to provide a preparation method of efficient and durable anti-mite mosaic spinning yarn, the application prepares the nano-scale microcapsule with adjustable particle size special for mosaic spinning so as to realize efficient and durable anti-mite effect of fabrics, and the application prepares the anti-mite microcapsule and regulates the particle size so as to be suitable for mosaic spinning and obtain comfortable and durable cotton yarn with durable anti-mite effect.
The application relates to a preparation method of anti-mite inlay spun yarn, which comprises the following steps:
(1) Preparing an anti-mite microcapsule, wherein the core material of the anti-mite microcapsule contains oily anti-mite agent, and the wall material is calcium alginate;
(2) Mixing the high polymer, the solvent and the anti-mite microcapsule uniformly to obtain spinning solution, and preparing cotton, carding cotton, drawing and spinning according to the spinning quality requirement, wherein an electrostatic spinning device is additionally arranged between a cotton stripping device and a drawing device for electrostatic spinning in the cotton carding stage, so that the embedding implantation of the micro-capsule anti-mite submicron fiber in a cotton web is completed, and the anti-mite embedded spun yarn is obtained.
The preferred mode of the preparation method is as follows:
the microcapsule wall material is made of calcium alginate material, has a cross-linked network structure, has good chemical stability and embedding efficiency, and can form a slow-release system, prolong the action time and facilitate the load of submicron fibers on the anti-mite agent when being prepared into the anti-mite microcapsule.
The microcapsule wall material is prepared by one of a sharp hole-coagulation bath method, a spray drying method, a complex coacervation method, an interfacial polymerization method and an in-situ polymerization method.
Preferably, the calcium alginate wall material of the anti-mite microcapsule is prepared from sodium alginate and calcium chloride by an orifice-coagulation bath method. The principle of microcapsule formation is as follows: calcium ions in a calcium chloride solution are selected as a cross-linking agent, and a cross-linking network is formed among sodium alginate molecular chains by utilizing an ion cross-linking reaction principle, so that the structure of the sodium alginate molecular chains is converted, and the core material anti-mite agent is encapsulated.
Further preferably, the preparation method of the anti-mite microcapsule in the step (1) comprises the following steps: adding an emulsifying agent, an auxiliary emulsifying agent and an aqueous sodium alginate solution into an oily anti-mite agent, pre-emulsifying to obtain a pre-emulsion, and then performing ice bath emulsification to obtain an emulsion; and (3) dropwise adding the emulsion into a cross-linking agent stirred in a water bath, reacting to obtain an anti-mite microcapsule suspension, stirring, solidifying, centrifugally washing, and freeze-drying to obtain the anti-mite microcapsule.
The oily anti-mite agent is one or more of natural plant essential oil (such as oleum Caryophylli, oleum Lavandula Angustifolia, oleum Eucalypti, cypress leaf oil, and citrus essential oil), eugenol (such as methyl eugenol and isoeugenol), and aromatic carboxylic acid ester (such as benzyl benzoate, methyl phenylacetate, and isoamyl salicylate);
the emulsifier is Tween-80; the auxiliary emulsifier is absolute ethyl alcohol; the adding amount of the oily anti-mite agent in the emulsion is 0.4-1.4 wt%, the concentration range of the sodium alginate aqueous solution is 0.02-0.1 wt%, the mass of the emulsifier is 1/30-1/6 of that of the oily anti-mite agent, and the mass ratio of the auxiliary emulsifier to the emulsifier is 1:2.
The ice bath emulsification time is 5-20 min;
the cross-linking agent is calcium chloride solution with the concentration of 0.06-0.2 wt%; the dropping rate of the emulsion is 0.1-0.5 mL/min; the stirring speed of the water bath is 600-1400 rpm; the reaction temperature is 15-60 ℃.
The grain diameter of the anti-mite microcapsule in the step (1) is 200-700 nm.
The step (1) is characterized in that the coating effect of the submicron fiber is poor due to the fact that the particle size of the microcapsule is too large, so that the microcapsule is exposed outside the fiber, the microcapsule is easy to damage or fall off, the durability is poor, and the process requirement is high due to the fact that the particle size is too small, and the production is not facilitated.
The high polymer in the step (2) is one or more of polyacrylonitrile PAN, polyurethane PU, cellulose acetate CA, polylactic acid PLA and polyvinyl alcohol PVA; the solvent is one or more of N, N-dimethylformamide DMF, acetone, acetic acid and deionized water.
The mass ratio of the high polymer to the solvent in the step (2) is 1:6-1:12.
Further, the mass ratio of the polymer to the solvent in the step (2) is one of 1:6, 1:7, 1:8, 1:9, 1:10, 1:11 and 1:12; the addition amount of the anti-mite microcapsule is 1/12-1/4 of the mass of PAN.
The electrostatic spinning process parameters in the step (2) are as follows: the environment temperature is 18-28 ℃, the relative humidity is 35-70%, the vertical height of the electrostatic spinning nozzle from the cotton web is 15-30 cm, and the applied voltage is 40-65 kV.
The anti-mite inlay spun yarn prepared by the method is provided.
The particle size of the traditional microcapsule is in the micron level, submicron fibers are difficult to completely coat, the particle size of the microcapsule is effectively controlled by adjusting various technological parameters, the anti-mite microcapsule with the particle size of nanometer scale (200-700 nm) is prepared, and the submicron fibers wrapping the anti-mite microcapsule are obtained through an electrostatic forming technology, so that the anti-mite microcapsule is prevented from falling off. And then used in inlay spinning to be compounded with cotton fibers.
Advantageous effects
The mode of coating the anti-mite agent by the microcapsule is adopted to prevent the anti-mite agent from suddenly releasing, so as to realize the lasting stability of the anti-mite effect. The particle size of the microcapsule is effectively controlled by adjusting different technological parameters, so that the microcapsule is in a nano-scale range (200-700 nm) to be matched with the fineness of submicron fibers, the complete package of the fiber to the microcapsule is realized, the microcapsule can be applied to inlay spinning, and the submicron fibers wrapping the anti-mite microcapsule are further coated by cotton fibers by utilizing the scale difference of the diameters of the submicron fibers and the cotton fibers. The nanometer microcapsule with controllable particle size is prepared and used in inlay spinning, so that the washing resistance, the controlled release property of the anti-mite agent and the durable durability of the final product can be enhanced, a better anti-mite effect can be obtained, and the softness and skin-friendly comfort of cotton fabrics can be maintained.
Drawings
FIG. 1 is a profile of the apparent morphology and diameter of the microcapsules of example 4, wherein (a) is a 9k magnification apparent morphology; (b) an apparent topography at a magnification of 100 k; (c) is a microcapsule diameter profile;
FIG. 2 is a morphology of the microcapsule-loaded sub-micrometer fibers, wherein (a) is a morphology of the nano-scale microcapsule-loaded sub-micrometer fibers of example 4 and (b) is a morphology of the micro-scale microcapsule-loaded sub-micrometer fibers of example 5;
FIG. 3 is an apparent topography of the inlay spun anti-mite yarn prepared in example 4, wherein (a) is a yarn apparent topography at magnification of 150 and (b) is a yarn apparent topography at magnification of 700;
fig. 4 is the retention of the anti-mite agent for 21 days for the benzyl benzoate/calcium alginate microcapsules and the inlay spun yarn prepared in example 4.
Detailed Description
The application will be further illustrated with reference to specific examples. It is to be understood that these examples are illustrative of the present application and are not intended to limit the scope of the present application. Furthermore, it should be understood that various changes and modifications can be made by one skilled in the art after reading the teachings of the present application, and such equivalents are intended to fall within the scope of the application as defined in the appended claims.
Benzyl benzoate (benzyl benzoate) (beijing enokic technologies limited); tween-80 (national pharmaceutical group chemicals limited); sodium alginate (Shanghai Ala Biochemical technologies Co., ltd.); calcium chloride (national pharmaceutical group chemical agents limited); polyacrylonitrile (PAN, mw=85000, shanghai gold mountain petrochemical company limited); n, N-dimethylformamide (DMF, national pharmaceutical group chemical company limited); deionized water
Example 1
S1: preparing sodium alginate aqueous solution with the concentration of 0.4mg/mL, and stirring the sodium alginate aqueous solution for 10 hours at normal temperature until the sodium alginate aqueous solution is completely dissolved. 0.6g of benzyl benzoate is weighed, an emulsifier Tween-80 and an auxiliary emulsifier absolute ethyl alcohol are added into the benzyl benzoate, then 100mL of sodium alginate aqueous solution is added into the mixture to serve as a water phase, and the mixture is stirred for 30min for pre-emulsification, wherein the mass of the emulsifier is 1/10 of that of the benzyl benzoate, and the mass ratio of the absolute ethyl alcohol to the Tween-80 is 1:2.
S2: and (3) placing the pre-emulsion of benzyl benzoate in an ice bath for emulsification in a cell pulverizer, and adjusting the emulsification time to 10min.
S3: preparing CaCl with concentration of 1.2mg/mL 2 Aqueous solution and weighing the same amount of CaCl as benzyl benzoate emulsion 2 Stirring the aqueous solution in a water bath in a beaker, and then dripping the emulsified white benzyl benzoate emulsion into CaCl at a certain rate 2 In an aqueous solution. Wherein the reaction temperature is 45 ℃, the stirring speed is 1200rpm, and the dripping speed is controlled to be 0.2mL/min, so as to obtain the anti-mite microcapsule suspension.
S4: the solution was stirred to cure for 30min. After solidification, loading the product suspension into a centrifuge tube, setting the rotating speed to 6000rpm, washing and centrifuging for 3 times, taking the bottom sediment, and carrying out freeze drying treatment on the bottom sediment for 24 hours to obtain benzyl benzoate/calcium alginate microcapsule powder with the particle size of 251 nm.
S5: 7.2g of PAN was dissolved in 51.6g of DMF, 1.2g of the anti-mite microcapsule prepared in step S4 was added thereto, and the mixed solution was stirred uniformly on a magnetic stirrer to obtain a polyelectrolyte spinning solution. The manufacturing of the inlaid anti-mite yarn is carried out through the procedures of cotton matching, cotton carding, drawing, roving and ring spinning. In the carding process, a cotton web is used as a receiving device for electrostatic spinning, and the adopted spinning process parameters are that the ambient temperature is 25 ℃, the relative humidity is 55%, and the spinning voltage is 45kV. And then preparing the anti-mite inlay spinning yarn through a subsequent process.
Example 2
S1: preparing sodium alginate aqueous solution with the concentration of 0.2mg/mL, and stirring the sodium alginate aqueous solution for 10 hours at normal temperature until the sodium alginate aqueous solution is completely dissolved. 0.6g of benzyl benzoate is weighed, an emulsifier Tween-80 and an auxiliary emulsifier absolute ethyl alcohol are added into the benzyl benzoate, then 100mL of sodium alginate aqueous solution is added into the mixture to serve as a water phase, and the mixture is stirred for 30min for pre-emulsification, wherein the mass of the emulsifier is 1/10 of that of the benzyl benzoate, and the mass ratio of the absolute ethyl alcohol to the Tween-80 is 1:2.
S2: and (3) placing the pre-emulsion of benzyl benzoate in an ice bath for emulsification in a cell pulverizer, and adjusting the emulsification time to 10min.
S3: preparing CaCl with concentration of 0.6mg/mL 2 Aqueous solution and weighing the same amount of CaCl as benzyl benzoate emulsion 2 Stirring the aqueous solution in a water bath in a beaker, and then dripping the emulsified white benzyl benzoate emulsion into CaCl at a certain rate 2 In an aqueous solution. Wherein the reaction temperature is 45 ℃, the stirring speed is 1200rpm, and the dripping speed is controlled to be 0.2mL/min, so as to obtain the anti-mite microcapsule suspension.
S4: the solution was stirred to cure for 30min. After solidification, loading the product suspension into a centrifuge tube, setting the rotating speed to 6000rpm, washing and centrifuging for 3 times, taking the bottom sediment, and carrying out freeze drying treatment on the bottom sediment for 24 hours to obtain benzyl benzoate/calcium alginate microcapsule powder with the particle size of 385 nm.
S5: 7.2g of PAN was dissolved in 51.6g of DMF, 1.2g of the anti-mite microcapsule prepared in step S4 was added thereto, and the mixed solution was stirred uniformly on a magnetic stirrer to obtain a polyelectrolyte spinning solution. The manufacturing of the inlaid anti-mite yarn is carried out through the procedures of cotton matching, cotton carding, drawing, roving and ring spinning. In the carding process, a cotton web is used as a receiving device for electrostatic spinning, and the adopted spinning process parameters are that the ambient temperature is 25 ℃, the relative humidity is 55%, and the spinning voltage is 45kV. And then preparing the anti-mite inlay spinning yarn through a subsequent process.
Example 3
S1: preparing sodium alginate aqueous solution with the concentration of 0.4mg/mL, and stirring the sodium alginate aqueous solution for 10 hours at normal temperature until the sodium alginate aqueous solution is completely dissolved. 0.6g of benzyl benzoate is weighed, an emulsifier Tween-80 and an auxiliary emulsifier absolute ethyl alcohol are added into the benzyl benzoate, then 100mL of sodium alginate aqueous solution is added into the mixture to serve as a water phase, and the mixture is stirred for 30min for pre-emulsification, wherein the mass of the emulsifier is 1/6 of that of the benzyl benzoate, and the mass ratio of the absolute ethyl alcohol to the Tween-80 is 1:2.
S2: and (3) placing the pre-emulsion of benzyl benzoate in an ice bath for emulsification in a cell pulverizer, and adjusting the emulsification time to 5min.
S3: preparing CaCl with concentration of 1.2mg/mL 2 Aqueous solution and weighing the same amount of CaCl as benzyl benzoate emulsion 2 The aqueous solution was stirred in a beaker in a water bath and the emulsified white benzyl benzoate was then addedEster emulsion, dropping CaCl at a certain rate 2 In an aqueous solution. Wherein the reaction temperature is 45 ℃, the stirring speed is 1200rpm, and the dripping speed is controlled to be 0.2mL/min, so as to obtain the anti-mite microcapsule suspension.
S4: the solution was stirred to cure for 30min. After solidification, loading the product suspension into a centrifuge tube, setting the rotating speed to 6000rpm, washing and centrifuging for 3 times, taking the bottom sediment, and carrying out freeze drying treatment on the bottom sediment for 24 hours to obtain benzyl benzoate/calcium alginate microcapsule powder with the particle size of 305 nm.
S5: 7.2g of PAN was dissolved in 51.6g of DMF, 1.2g of the anti-mite microcapsule prepared in step S4 was added thereto, and the mixed solution was stirred uniformly on a magnetic stirrer to obtain a polyelectrolyte spinning solution. The manufacturing of the inlaid anti-mite yarn is carried out through the procedures of cotton matching, cotton carding, drawing, roving and ring spinning. In the carding process, a cotton web is used as a receiving device for electrostatic spinning, and the adopted spinning process parameters are that the ambient temperature is 25 ℃, the relative humidity is 55%, and the spinning voltage is 45kV. And then preparing the anti-mite inlay spinning yarn through a subsequent process.
Example 4
S1: preparing sodium alginate aqueous solution with the concentration of 0.4mg/mL, and stirring the sodium alginate aqueous solution for 10 hours at normal temperature until the sodium alginate aqueous solution is completely dissolved. 0.6g of benzyl benzoate is weighed, an emulsifier Tween-80 and an auxiliary emulsifier absolute ethyl alcohol are added into the benzyl benzoate, then 100mL of sodium alginate aqueous solution is added into the mixture to serve as a water phase, and the mixture is stirred for 30min for pre-emulsification, wherein the mass of the emulsifier is 1/10 of that of the benzyl benzoate, and the mass ratio of the absolute ethyl alcohol to the Tween-80 is 1:2.
S2: and (3) placing the pre-emulsion of benzyl benzoate in an ice bath for emulsification in a cell pulverizer, and adjusting the emulsification time to 10min.
S3: preparing CaCl with concentration of 1.2mg/mL 2 Aqueous solution and weighing the same amount of CaCl as benzyl benzoate emulsion 2 Stirring the aqueous solution in a water bath in a beaker, and then dripping the emulsified white benzyl benzoate emulsion into CaCl at a certain rate 2 In an aqueous solution. Wherein the reaction temperature is 30 ℃, the stirring speed is 1400rpm, and the dripping speed is controlled to be 0.1mL/min, thus obtaining the anti-rust agentMite microcapsule suspension.
S4: the solution was stirred to cure for 30min. After solidification, loading the product suspension into a centrifuge tube, setting the rotating speed to 6000rpm, washing and centrifuging for 3 times, taking the bottom sediment, and carrying out freeze drying treatment on the bottom sediment for 24 hours to obtain benzyl benzoate/calcium alginate microcapsule powder with the particle size of 432 nm.
S5: 7.2g of PAN was dissolved in 51.6g of DMF, 1.2g of the anti-mite microcapsule prepared in step S4 was added thereto, and the mixed solution was stirred uniformly on a magnetic stirrer to obtain a polyelectrolyte spinning solution. The manufacturing of the inlaid anti-mite yarn is carried out through the procedures of cotton matching, cotton carding, drawing, roving and ring spinning. In the carding process, a cotton web is used as a receiving device for electrostatic spinning, and the adopted spinning process parameters are that the ambient temperature is 25 ℃, the relative humidity is 55%, and the spinning voltage is 45kV. And then preparing the anti-mite inlay spinning yarn through a subsequent process.
Example 5
S1: preparing sodium alginate aqueous solution with the concentration of 0.4mg/mL, and stirring the sodium alginate aqueous solution for 10 hours at normal temperature until the sodium alginate aqueous solution is completely dissolved. 0.6g of benzyl benzoate is weighed, an emulsifier Tween-80 and an auxiliary emulsifier absolute ethyl alcohol are added into the benzyl benzoate, then 100mL of sodium alginate aqueous solution is added into the mixture to serve as a water phase, and the mixture is stirred for 30min for pre-emulsification, wherein the mass of the emulsifier is 1/30 of that of the benzyl benzoate, and the mass ratio of the absolute ethyl alcohol to the Tween-80 is 1:2.
S2: and (3) placing the pre-emulsion of benzyl benzoate in an ice bath for emulsification in a cell pulverizer, and adjusting the emulsification time to 20min.
S3: preparing CaCl with concentration of 1.2mg/mL 2 Aqueous solution and weighing the same amount of CaCl as benzyl benzoate emulsion 2 Stirring the aqueous solution in a water bath in a beaker, and then dripping the emulsified white benzyl benzoate emulsion into CaCl at a certain rate 2 In an aqueous solution. Wherein the reaction temperature is 60 ℃, the stirring speed is 600rpm, and the dripping speed is controlled to be 0.5mL/min, so as to obtain the anti-mite microcapsule suspension.
S4: the solution was stirred to cure for 30min. After solidification, loading the product suspension into a centrifuge tube, setting the rotating speed to 6000rpm, washing and centrifuging for 3 times, taking the bottom sediment, and carrying out freeze drying treatment on the bottom sediment for 24 hours to obtain benzyl benzoate/calcium alginate microcapsule powder with the particle size of 2.9 mu m.
S5: 7.2g of PAN was dissolved in 51.6g of DMF, 1.2g of the anti-mite microcapsule prepared in step S4 was added thereto, and the mixed solution was stirred uniformly on a magnetic stirrer to obtain a polyelectrolyte spinning solution. The manufacturing of the inlaid anti-mite yarn is carried out through the procedures of cotton matching, cotton carding, drawing, roving and ring spinning. In the carding process, a cotton web is used as a receiving device for electrostatic spinning, and the adopted spinning process parameters are that the ambient temperature is 25 ℃, the relative humidity is 55%, and the spinning voltage is 45kV. And then preparing the anti-mite inlay spinning yarn through a subsequent process.
Performance tests were performed on examples 1 to 4, respectively. The apparent morphology of the yarn was observed using a scanning electron microscope, as shown in fig. 3, submicron fibers were present in the yarn body in the form of adhering to the surface of cotton fibers and filling in the pores of the cotton fibers, and the effect on the macroscopic morphology of the yarn was insignificant due to the dimensional difference between the two. The microcapsule and the mite-proof mosaic spun yarn are placed in a constant temperature environment at 25 ℃ for 21 days, 1/6 of the microcapsule is taken out from the first, the second, the third, the fourth, the fifth, the fourth and the fifth days respectively, the microcapsule and the mite-proof mosaic spun yarn are soaked in ethanol solution for ultrasonic treatment to extract the mite-proof agent into ethanol and test the content of the mite-proof agent, and the measured retention rates of the microcapsule and the mite-proof mosaic spun yarn are both above 90 percent, but the retention rate of the mite-proof agent of the mite-proof mosaic spun yarn is higher than that of the microcapsule. Taking the specific data of example 4 as an example, as shown in fig. 4, after the microcapsule and the anti-mite agent in the anti-mite inlay yarn are placed at a temperature of 25 ℃ for 21 days, the retention rates of the microcapsule and the anti-mite agent in the anti-mite inlay yarn are 93.5% and 96.2%, respectively, and it can be found that the anti-mite agent in the inlay yarn can be retained for a long time by multiple coating. In addition, the mite repellent performance of the yarn is tested by referring to GB/T24253-2009 evaluation of the anti-mite performance of textiles, and the mite repellent rate of the anti-mite inlay spun yarn prepared in examples 1-4 is above 90%, and in the example 4, the mite repellent rate can reach 97.79%, so that the product has better anti-mite effect.
Claims (10)
1. A preparation method of mite-proof inlay spun yarn comprises the following steps:
(1) Preparing an anti-mite microcapsule, wherein the core material of the anti-mite microcapsule contains oily anti-mite agent, and the wall material is calcium alginate;
(2) Mixing the high polymer, the solvent and the mite-proof microcapsules uniformly to obtain spinning solution, and preparing cotton, carding cotton, drawing and spinning according to the spinning quality requirement, wherein an electrostatic spinning device is additionally arranged between a cotton stripping device and a drawing device for electrostatic spinning in the cotton carding stage to obtain the mite-proof mosaic spinning yarn.
2. The method according to claim 1, wherein the microcapsule wall material is prepared by one of a sharp hole-coagulation bath method, a spray drying method, a complex coacervation method, an interfacial polymerization method and an in situ polymerization method.
3. The method of claim 1, wherein the method of preparing the anti-mite microcapsule in step (1) comprises: adding an emulsifying agent, an auxiliary emulsifying agent and an aqueous sodium alginate solution into an oily anti-mite agent, pre-emulsifying to obtain a pre-emulsion, and then performing ice bath emulsification to obtain an emulsion;
and (3) dropwise adding the emulsion into a cross-linking agent stirred in a water bath, reacting to obtain an anti-mite microcapsule suspension, stirring, solidifying, centrifugally washing, and freeze-drying to obtain the anti-mite microcapsule.
4. The method according to claim 3, wherein the oily anti-mite agent is one or more of natural plant essential oil, eugenol, and aromatic carboxylic ester; the emulsifier is Tween-80; the auxiliary emulsifier is absolute ethyl alcohol; the adding amount of the oily anti-mite agent in the emulsion is 0.4-1.4 wt%, the concentration range of the sodium alginate aqueous solution is 0.02-0.1 wt%, the mass of the emulsifier is 1/30-1/6 of that of the oily anti-mite agent, and the mass ratio of the auxiliary emulsifier to the emulsifier is 1:2.
5. The method according to claim 3, wherein the ice bath emulsification time is 5 to 20min; the cross-linking agent is calcium chloride solution with the concentration of 0.06-0.2 wt%; the dropping rate of the emulsion is 0.1-0.5 mL/min; the stirring speed of the water bath is 600-1400 rpm; the reaction temperature is 15-60 ℃.
6. The method according to claim 1, wherein the particle size of the anti-mite microcapsule in the step (1) is 200 to 700nm.
7. The preparation method according to claim 1, wherein the high polymer in the step (2) is one or more of polyacrylonitrile PAN, polyurethane PU, cellulose acetate CA, polylactic acid PLA, and polyvinyl alcohol PVA; the solvent is one or more of N, N-dimethylformamide DMF, acetone, acetic acid and deionized water.
8. The preparation method according to claim 1, wherein the mass ratio of the high polymer to the solvent in the step (2) is 1:6-1:12; the addition amount of the anti-mite microcapsule is 1/12-1/4 of the mass of PAN.
9. The method according to claim 1, wherein the electrostatic spinning process parameters in the step (2) are as follows: the environment temperature is 18-28 ℃, the relative humidity is 35-70%, the vertical height of the electrostatic spinning nozzle from the cotton web is 15-30 cm, and the applied voltage is 40-65 kV.
10. An anti-mite inlay spun yarn made by the method of claim 1.
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