CN113699793B - Gellable fiber material and preparation method thereof - Google Patents
Gellable fiber material and preparation method thereof Download PDFInfo
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- CN113699793B CN113699793B CN202111002092.3A CN202111002092A CN113699793B CN 113699793 B CN113699793 B CN 113699793B CN 202111002092 A CN202111002092 A CN 202111002092A CN 113699793 B CN113699793 B CN 113699793B
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- D06M15/00—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment
- D06M15/01—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment with natural macromolecular compounds or derivatives thereof
- D06M15/03—Polysaccharides or derivatives thereof
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- D06M10/00—Physical treatment of fibres, threads, yarns, fabrics, or fibrous goods made from such materials, e.g. ultrasonic, corona discharge, irradiation, electric currents, or magnetic fields; Physical treatment combined with treatment with chemical compounds or elements
- D06M10/02—Physical treatment of fibres, threads, yarns, fabrics, or fibrous goods made from such materials, e.g. ultrasonic, corona discharge, irradiation, electric currents, or magnetic fields; Physical treatment combined with treatment with chemical compounds or elements ultrasonic or sonic; Corona discharge
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- D06M13/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment
- D06M13/10—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment with compounds containing oxygen
- D06M13/184—Carboxylic acids; Anhydrides, halides or salts thereof
- D06M13/188—Monocarboxylic acids; Anhydrides, halides or salts thereof
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- D06M13/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment
- D06M13/10—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment with compounds containing oxygen
- D06M13/184—Carboxylic acids; Anhydrides, halides or salts thereof
- D06M13/207—Substituted carboxylic acids, e.g. by hydroxy or keto groups; Anhydrides, halides or salts thereof
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- D06M15/00—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment
- D06M15/01—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment with natural macromolecular compounds or derivatives thereof
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- D06M15/00—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment
- D06M15/19—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment with synthetic macromolecular compounds
- D06M15/21—Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
- D06M15/327—Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds of unsaturated alcohols or esters thereof
- D06M15/333—Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds of unsaturated alcohols or esters thereof of vinyl acetate; Polyvinylalcohol
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- D06M23/00—Treatment of fibres, threads, yarns, fabrics or fibrous goods made from such materials, characterised by the process
- D06M23/12—Processes in which the treating agent is incorporated in microcapsules
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- D06M2101/00—Chemical constitution of the fibres, threads, yarns, fabrics or fibrous goods made from such materials, to be treated
- D06M2101/02—Natural fibres, other than mineral fibres
- D06M2101/04—Vegetal fibres
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- D06M2101/00—Chemical constitution of the fibres, threads, yarns, fabrics or fibrous goods made from such materials, to be treated
- D06M2101/02—Natural fibres, other than mineral fibres
- D06M2101/04—Vegetal fibres
- D06M2101/06—Vegetal fibres cellulosic
- D06M2101/08—Esters or ethers of cellulose
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- D06M2101/00—Chemical constitution of the fibres, threads, yarns, fabrics or fibrous goods made from such materials, to be treated
- D06M2101/16—Synthetic fibres, other than mineral fibres
- D06M2101/30—Synthetic polymers consisting of macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
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- D06M2200/00—Functionality of the treatment composition and/or properties imparted to the textile material
- D06M2200/40—Reduced friction resistance, lubricant properties; Sizing compositions
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Abstract
The invention discloses a gellable fiber material and a preparation method thereof, and belongs to the technical field of textile fibers. The invention obtains a natural degradable fiber material with gel function by taking a chitosan material containing microcapsules as a sizing agent and carrying out post-treatment on the basis of degradable cellulose fibers, protein fibers, polylactic acid fibers, polycaprolactone fibers, polyglycolide fibers and the like without adding any cross-linking agent. The preparation method disclosed by the invention is simple in process and easy to operate, and the developed gel-able fiber material is controllable in gel process and has a potential application prospect in the field of medical makeup.
Description
Technical Field
The invention belongs to the technical field of textile fibers, and particularly relates to a gel-capable fiber material and a preparation method thereof.
Background
The hydrogel is a novel functional polymer material with environmental sensitivity responsiveness, high absorbability and slow release. Hydrogel fibers not only have the above-described characteristics, but also possess a fibrous or fibrous appearance. The appearance of the fiber increases the specific surface area and the length-diameter ratio, and not only improves the properties of swelling property, slow release property, immobilization capacity and the like of the hydrogel fiber, but also endows the hydrogel fiber with a plurality of new applications. These characteristics make the hydrogel fiber have very bright prospect in the fields of tissue engineering, biomedicine, textile, high polymer materials and the like. The chitosan has multiple physiological functions of biodegradability, biocompatibility, nontoxicity, bacteriostasis, cancer resistance, lipid reduction, immunity enhancement and the like, so the hydrogel of the chitosan has great application potential.
The existing intelligent hydrogel fiber is a soft and wet material consisting of responsive macromolecules and water, can respond to external temperature, light, pH and electromagnetic field stimulation, and generates gel with the shape change of volume, length, diameter and the like. Patent CN109999221A discloses an oriented chitosan fiber hydrogel and a preparation method thereof, and the fiber hydrogel obtained by the method is prepared from single-component chitosan. Dissolving 0.5-4% of chitosan in an acetic acid aqueous solution, uniformly mixing with 0.2-0.6% of polyethylene oxide (PEO) aqueous solution, then carrying out electrostatic spinning, receiving the spun fiber by 0.5-3% of sodium tripolyphosphate receiving solution, carrying out rotary collection on the crosslinked chitosan fiber to obtain an oriented fiber bundle, and finally grafting functional polypeptide onto the fiber, wherein the fiber has a gel function. Patent CN101624778A discloses a method for producing high water absorption chitosan fiber, which comprises soaking chitosan fiber in ethanol for 30-60 min, dewatering, then placing into succinic anhydride ethanol solution with pH of 2-6 for 5-120 min, then placing into mixed solution of polysorbate (Tween) series surfactant and absolute ethyl alcohol for soaking, dewatering and airing, and the prepared chitosan fiber has the characteristic of being gelled when meeting water. At present, chitosan gel is mostly realized by adding acid, but the method has the defects of uncontrollable acidic pH, poor gel stability and the like.
Most of hydrogel fibers at the present stage are single response or double response, most of the hydrogel fibers are added with a chemical cross-linking agent in the preparation process, the preparation process is complicated, the cost is high, and the functionality of the hydrogel fibers cannot be embodied more flexibly.
Disclosure of Invention
The invention aims to provide a method for producing gelation-controllable hydrogel fibers without adding a cross-linking agent, aiming at the problems that the production cost of the hydrogel fibers in the prior art is high, the use conditions are limited, and the degradation is incomplete due to the addition of micromolecule substances such as the cross-linking agent and the like into the materials during the production of the hydrogel fibers; the heat-sensitive or pressure-sensitive microcapsules are added into the sizing agent, so that the release of weak acid in the microcapsules can be controlled, and the product can be more conveniently and flexibly gelatinized and is more convenient to use; the pretreatment fiber and sizing material adopted by the method, including the microcapsule, can be naturally degraded, are harmless to human bodies, and are green and environment-friendly.
In order to achieve the purpose, the invention can be realized by adopting the following technical scheme:
a method of preparing a gellable fibrous material comprising the steps of:
s1, subjecting any biodegradable fiber such as cellulose fiber, protein fiber, polylactic acid fiber, polycaprolactone fiber, polyglycolide fiber and the like to plasma treatment to obtain pretreated fiber;
s2, dissolving chitosan in water, acetic acid, hydrochloric acid and benzoic acid solution or preparing chitosan emulsion, performing vacuum defoaming treatment to prepare a chitosan sizing agent, and mixing acid-containing microcapsules into the sizing agent;
and S3, soaking the pretreated fiber after the plasma treatment into a chitosan sizing agent, uniformly sizing, and drying to obtain the gel fiber material.
According to the present invention, the pretreated fiber in step S1 can be, but not limited to, the above fiber, any natural degradable fiber product, and besides, the pretreated fiber can also be any synthetic fiber such as polyester fiber, nylon fiber, acrylic fiber, vinylon fiber, etc., and such fiber can also be used for the preparation of sizing gel fiber, but will lose the natural degradation property.
Preferably, in step S1, the cellulose fibers are fibers such as viscose, tencel, modal, cuprammonium, acetate, etc.; the protein fiber is silk, soybean protein fiber, milk fiber, gelatin fiber, etc.
Preferably, in step S1, the plasma treatment conditions are: the gas is nitrogen, the processing power is 100 to 300W, the pressure is 5 to 60Pa, and the processing time is 5 to 60min. The surface of the fiber is rough by the plasma treatment, so that the chitosan slurry containing the microcapsules can be easily attached to the surface.
Preferably, in the step S2, the content of chitosan in the chitosan sizing agent is 1-10% w/v, and the content of acid-containing microcapsules is 1-15% w/v. Too small a proportion, low slurry viscosity, low sizing rate and poor fiber gelling effect, and too large a proportion, high slurry viscosity, poor slurry permeability, unfavorable sizing and relatively poor fiber gelling effect.
Preferably, in step S2, the core material of the acid-containing microcapsule is any nontoxic acidic material such as acetic acid, lactic acid, mandelic acid, malic acid, citric acid, tartaric acid, glycolic acid, salicylic acid, hyaluronic acid, pantothenic acid, nicotinic acid, tranexamic acid, ascorbic acid, ferulic acid, and the wall material is a thermosensitive and pressure-sensitive material such as starch, polyvinyl alcohol, polyvinylpyrrolidone, gelatin, cyclodextrin, xanthan gum, pectin, agar, and the like.
Preferably, in the step S3, the pretreated fiber is soaked in a chitosan sizing agent at the soaking temperature of 20-80 ℃ for 0.5-50min.
Preferably, in the step S3, the drying temperature is 30-80 ℃ and the time is 0.5-3h.
The implementation of the gel-able fiber material and the preparation method thereof has the following beneficial effects:
1. the method is prepared from biodegradable materials, is green and environment-friendly, has no pollution to the environment, is easy to obtain raw materials, is low in price, and can further expand the application range of the materials.
2. The gel fiber prepared by the method can be completely degraded without adding any chemical cross-linking agent, and has the advantages of low cost, quick production process, simple operation and easy realization of continuous production.
3. The invention provides that microcapsules are added into spinning solution, different response stimulation types are given to fibers by utilizing microcapsules with different functions, and the method can also be used for producing other intelligent functional materials.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1
A gellable fiber material and a preparation method thereof comprise the following steps:
(1) Firstly, carrying out plasma treatment on acetate fibers under the conditions that nitrogen is adopted as gas, the treatment power is 100W, and the pressure is 5Pa, wherein the treatment time is 60min, and obtaining the pretreated fibers.
(2) Then, chitosan with the content of 1% (w/v) is dissolved in deionized water, and the chitosan sizing agent is prepared through vacuum defoaming treatment, and microcapsules with acetic acid as a core material and polyvinyl alcohol as a wall material are mixed into the sizing agent at the same time, wherein the addition amount is 1% (w/v).
(3) And soaking the pretreated fiber after the plasma treatment into a chitosan sizing agent at the soaking temperature of 20 ℃ for 50min, uniformly sizing, and then drying in a drying oven at the temperature of 30 ℃ for 0.5h to obtain the gel-able fiber material.
The prepared gel fiber is put into hot water with the temperature of more than 65 ℃, pressure is applied to the fiber or the fiber is placed in an acid environment, the fiber is gradually gelated, and self-gelation can be realized.
Example 2
A gellable fiber material and a preparation method thereof comprise the following steps:
(1) Firstly, carrying out plasma treatment on the soybean protein fiber under the conditions that nitrogen is adopted as gas, the treatment power is 300W, and the pressure is 60Pa, wherein the treatment time is 5min, and obtaining the pretreated fiber.
(2) Then, chitosan with the content of 10% (w/v) is dissolved in hydrochloric acid, and the chitosan sizing agent is prepared through vacuum defoaming treatment, wherein the core material of the chitosan sizing agent is citric acid, the wall material of the chitosan sizing agent is gelatin microcapsule, and the addition amount of the chitosan sizing agent is 15% (w/v).
(3) And soaking the pretreated fiber after the plasma treatment into a chitosan sizing agent at the soaking temperature of 30 ℃ for 0.5min, uniformly sizing, and drying in a drying oven at the temperature of 30 ℃ for 3h to obtain the gel-able fiber material.
Putting the fibers on the prepared chitosan into an environment with the temperature of more than 40 ℃, applying pressure to the fibers or placing the fibers in an acid environment, and gradually gelatinizing the fibers to realize self-gelation.
Example 3
A gellable fiber material and a preparation method thereof comprise the following steps:
(1) Firstly, carrying out plasma treatment on polylactic acid fibers under the conditions that gas adopts nitrogen, the treatment power is 200W, and the pressure is 35Pa, wherein the treatment time is 30min, and obtaining the pretreated fibers.
(2) Then, chitosan with the content of 6% (w/v) is dissolved in benzoic acid, and the chitosan sizing agent is prepared through vacuum defoaming treatment, wherein the core material is acetic acid, the wall material is starch microcapsule, and the addition amount is 8% (w/v).
(3) And soaking the pretreated fiber after the plasma treatment into a chitosan sizing agent at the soaking temperature of 50 ℃ for 50min, uniformly sizing, and drying in a drying oven at the temperature of 55 ℃ for 2h to obtain the gellable fiber material.
Putting the fibers on the prepared chitosan into an environment with the temperature of more than 60 ℃, applying pressure to the fibers or placing the fibers in an acid environment, and gradually gelatinizing the fibers to realize self-gelation.
Example 4
A gellable fiber material and a preparation method thereof comprise the following steps:
(1) Firstly, carrying out plasma treatment on viscose fibers under the conditions that gas adopts nitrogen, the treatment power is 200W, and the pressure is 50Pa, wherein the treatment time is 20min, and obtaining the pretreated fibers.
(2) Then, chitosan with the content of 6% (w/v) is dissolved in acetic acid solution, and the chitosan sizing agent is prepared through vacuum defoaming treatment, wherein the core material of the chitosan sizing agent is acetic acid, the wall material of the chitosan sizing agent is a microcapsule of polyvinylpyrrolidone, and the addition amount of the chitosan sizing agent is 10% (w/v).
(3) And soaking the pretreated fiber after the plasma treatment into a chitosan sizing agent at the soaking temperature of 80 ℃ for 25min, uniformly sizing, and drying in a drying oven at the temperature of 80 ℃ for 0.5h to obtain the gel-able fiber material.
Putting the fibers on the prepared chitosan into normal-temperature water, putting the chitosan in an environment with the temperature of more than 130 ℃, applying pressure to the fibers or putting the chitosan in an acid environment, and gradually gelatinizing the fibers to realize self-gelation.
Example 5
A gellable fiber material and a preparation method thereof comprise the following steps:
(1) Firstly, carrying out plasma treatment on polyglycolide fibers under the conditions of adopting nitrogen gas as gas, treating power of 300W and pressure of 60Pa for 20min to obtain pretreated fibers.
(2) Then, chitosan with the content of 6% (w/v) is dissolved in an acetic acid solution, and a chitosan sizing agent is prepared through vacuum defoaming treatment, wherein the core material of the chitosan sizing agent is acetic acid, the wall material of the chitosan sizing agent is agar, and the addition amount of the chitosan sizing agent is 6% (w/v).
(3) And soaking the pretreated fiber after the plasma treatment into a chitosan sizing agent at the soaking temperature of 40 ℃ for 15min, uniformly sizing, and drying in a drying oven at the temperature of 45 ℃ for 1.5h to obtain the gel-able fiber material.
Putting the fibers on the prepared chitosan into an environment with the temperature of more than 60 ℃, applying pressure to the fibers or placing the fibers in an acid environment, and gradually gelatinizing the fibers to realize self-gelation.
Comparative example 1
A gellable fiber material and a preparation method thereof comprise the following steps:
(1) Firstly, carrying out plasma treatment on tencel fiber under the conditions that gas adopts nitrogen, the treatment power is 100W and the pressure is 50Pa, wherein the treatment time is 20min, and obtaining the pretreated fiber.
(2) Then, chitosan with the content of 6% (w/v) is dissolved in acetic acid solution, and the chitosan sizing agent is prepared through vacuum defoaming treatment.
(3) And soaking the pretreated fiber after the plasma treatment into a chitosan sizing agent at the soaking temperature of 30 ℃ for 25min, uniformly sizing, and drying in a drying oven at the temperature of 80 ℃ for 1h to obtain the gellable fiber material.
The fiber is put on the prepared chitosan in an environment with the temperature of more than 60 ℃, the fiber can not be gradually gelatinized when pressure is applied to the fiber, and the chitosan can be gelatinized when put in an acid environment.
Comparative example 2
A gellable fiber material and a preparation method thereof comprise the following steps:
(1) Firstly, carrying out plasma treatment on polyglycolide fiber under the conditions that gas adopts nitrogen, the treatment power is 250W, and the pressure is 30Pa, wherein the treatment time is 20min, and obtaining the pretreated fiber.
(2) Then, chitosan with the content of 2.5 percent (w/v) is dissolved in acetic acid solution, and the chitosan sizing agent is prepared through vacuum defoaming treatment.
(3) And soaking the pretreated fiber after the plasma treatment into a chitosan sizing agent at the soaking temperature of 30 ℃ for 35min, uniformly sizing, and drying in a drying oven at the temperature of 50 ℃ for 2h to obtain the gel-able fiber material.
The fibers on the prepared chitosan are put into an environment with the temperature of more than 40 ℃, the fibers can not be gradually gelatinized by applying pressure to the fibers, and the fibers can be gelatinized by putting into an acid environment.
The chitosan sizing fiber prepared by the method has the special functions of good air permeability, hygroscopicity and moisture retention, biocompatibility, no antigenicity, biodegradability, broad-spectrum antibacterial property, corrosion resistance, hemostasis, wound healing promotion and the like, and has very bright prospects in the fields of tissue engineering, biomedicine, textile, high polymer materials and the like.
Claims (6)
1. A method for preparing a gellable fiber material, comprising: the method comprises the following steps:
s1, treating biodegradable fibers in plasma to obtain pretreated fibers;
the plasma treatment conditions are as follows: adopting nitrogen as gas, processing power is 100 to 300W, pressure is 5 to 60Pa, and processing time is 5 to 60min;
s2, preparing chitosan into a solution or a chitosan emulsion, performing vacuum defoaming treatment to prepare a chitosan sizing agent, and mixing acid-containing microcapsules into the sizing agent;
dissolving chitosan in water, acetic acid solution, hydrochloric acid solution or benzoic acid solution to prepare solution;
the chitosan sizing agent contains 1-10% w/v of chitosan and 1-15% w/v of acid-containing microcapsules;
the core material of the acid-containing microcapsule is acetic acid, lactic acid, mandelic acid, malic acid, citric acid, tartaric acid, glycolic acid, salicylic acid, hyaluronic acid, pantothenic acid, nicotinic acid, tranexamic acid, ascorbic acid or ferulic acid, and the wall material is starch, polyvinyl alcohol, polyvinylpyrrolidone, gelatin, cyclodextrin, xanthan gum, pectin or agar;
and S3, soaking the pretreated fiber after the plasma treatment into a chitosan sizing agent, uniformly sizing, and drying to obtain the gel fiber material.
2. The method of claim 1, wherein: the biodegradable fiber is cellulose fiber, protein fiber, polylactic acid fiber, polycaprolactone fiber or polyglycolide fiber.
3. The production method according to claim 2, characterized in that: the cellulose fiber is viscose fiber, tencel fiber, modal fiber, cuprammonium fiber or acetate fiber; the protein fiber is silk, soybean protein fiber, milk fiber or gelatin fiber.
4. The method of claim 1, wherein: in the step S3, the pretreated fiber is soaked in the chitosan sizing agent at the temperature of 20-80 ℃ for 0.5-50min.
5. The method of claim 1, wherein: in the step S3, the drying temperature is 30-80 ℃, and the time is 0.5-3h.
6. A gellable fibrous material obtained by the production method according to claim 1.
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102604149A (en) * | 2012-04-12 | 2012-07-25 | 上海华谊生物技术有限公司 | Three-dimensional chitosan hydrogel and preparation method thereof |
| CN103603195A (en) * | 2013-11-13 | 2014-02-26 | 安徽甲特生物科技有限公司 | Preparation method and application of ecological finishing agent used for cellulose and protein fiber fabrics |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102604149A (en) * | 2012-04-12 | 2012-07-25 | 上海华谊生物技术有限公司 | Three-dimensional chitosan hydrogel and preparation method thereof |
| CN103603195A (en) * | 2013-11-13 | 2014-02-26 | 安徽甲特生物科技有限公司 | Preparation method and application of ecological finishing agent used for cellulose and protein fiber fabrics |
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