CN109537271B - Graphene aerogel modified flame-retardant fabric based on microbubble template sol-gel method and preparation method thereof - Google Patents
Graphene aerogel modified flame-retardant fabric based on microbubble template sol-gel method and preparation method thereof Download PDFInfo
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- CN109537271B CN109537271B CN201811508184.7A CN201811508184A CN109537271B CN 109537271 B CN109537271 B CN 109537271B CN 201811508184 A CN201811508184 A CN 201811508184A CN 109537271 B CN109537271 B CN 109537271B
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M11/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising
- D06M11/73—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with carbon or compounds thereof
- D06M11/74—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with carbon or compounds thereof with carbon or graphite; with carbides; with graphitic acids or their salts
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M2200/00—Functionality of the treatment composition and/or properties imparted to the textile material
- D06M2200/30—Flame or heat resistance, fire retardancy properties
Abstract
The invention provides a graphene aerogel modified flame-retardant fabric based on a microbubble template sol-gel method and a preparation method thereof, and the preparation method comprises the following steps: adding alkyl polyglycoside and lauryl sodium sulfate into deionized water to obtain a foam precursor solution; adding the graphene oxide solution into DL-cysteine, and carrying out pre-heating reduction to obtain pre-reduced graphene oxide hydrosol; mixing the foam precursor solution and the pre-reduced graphene oxide hydrosol, placing the fabric in the mixture, shearing at a high speed to form stable foam on the surface of the fabric, taking out the fabric, quickly freezing, and cracking a foam film to prepare a partially reduced graphene oxide liquid crystal porous material; and unfreezing the partially reduced graphene oxide liquid crystal porous material at room temperature, heating to reduce, and freeze-drying to obtain the graphene aerogel modified flame-retardant fabric. According to the invention, the graphene aerogel is attached to the inside and the surface of the fabric, so that the textile fabric with light specific gravity, insolubility, no melting and excellent flame retardant property is prepared.
Description
Technical Field
The invention belongs to the technical field of textile materials, and particularly relates to a graphene aerogel modified flame-retardant fabric based on a microbubble template sol-gel method and a preparation method thereof.
Background
The graphene is a two-dimensional carbon nano-structure material which is allotrope with fullerene and carbon nano-tubes, and the unique two-dimensional nano-laminated carbon structure of the graphene enables the graphene to have ultrahigh specific surface area, electric conductivity, heat conductivity, antibacterial property and mechanical property, so that the graphene serving as an additive can endow the textile with functions of far infrared, ultraviolet resistance, antibacterial property, bacteriostasis, flame retardance, mechanical enhancement and the like, and the added value of the textile is improved.
The flammability of textiles has been the primary source of fire hazard, and therefore it is essential to have a flame retardant finish on textiles to prevent fires. The graphene has a two-dimensional staggered laminated structure, so that the graphene has a lamellar blocking effect, the heat transfer, the diffusion and overflow of pyrolysis products and the diffusion and mixing of oxygen can be delayed, and the graphene is low in toxicity, environment-friendly and halogen-free, so that the graphene modified flame-retardant textile has a good market prospect.
Chinese patent CN104630928B discloses a preparation method of a graphene-based reinforced flame-retardant regenerated polyester staple fiber, which comprises the steps of carrying out surface sulfonic acid group functionalization treatment on graphene, mixing the graphene with polyvinyl alcohol, polyvinylpyrrolidone and tetracyanodimethylbenzoquinone, stirring, dispersing, adding into polyester powder, and preparing graphene master batch by adopting a double-screw granulation process; mixing a reactive phosphorus halogen-free flame retardant with polyester powder, and preparing a phosphorus halogen-free flame retardant master batch by a screw granulation process; then carrying out vacuum mixing and drying on the graphene master batch, the phosphorus halogen-free flame-retardant master batch and the recycled polyester raw material at 90-140 ℃, pumping a melt obtained by melting the dried raw material under the action of a screw extruder into a homogenizing impurity removal stirrer through a melt pump for homogenization impurity removal treatment, then the melt is pumped to a secondary filter, the filtered melt enters a 275-278 ℃ spinning manifold after passing through a mixed melt arranged on a pipeline, spinning is carried out, the spun fiber is drawn, the graphene adopted in the method not only has a reinforcing effect on the polyester fiber, effectively improves the mechanical property of the fiber (the strength of the fiber is improved by 0.5-1.2 cN/dtex), has high thermal stability and high flame-retardant efficiency, can generate a synergistic flame-retardant effect with a phosphorus halogen-free flame retardant, effectively reduces the addition amount of the flame retardant, and reduces the cost. The fabric with the conductive flame-retardant coating and the preparation method thereof disclosed by Chinese patent CN106996035A are characterized in that 20-30mg/mL of graphene oxide hydrosol is coated on the surface of the fabric, the fabric is dried at 60-120 ℃ to obtain the fabric with the graphene oxide coating, then the fabric with the graphene oxide coating is soaked in sodium hydrosulfite and/or an aqueous solution of an L-ascorbic acid reducing agent, and a reduction reaction is carried out at 80-95 ℃ to reduce the graphene oxide into graphene, so that the fabric with the conductive flame-retardant coating is obtained. It is known from the above prior art that graphene can be added into fibers or coated on the surface of textiles to impart certain flame retardancy to the textiles. The graphene aerogel is a three-dimensional network formed by connecting graphene, has the characteristics of ultralow density, large pore volume, high specific surface area and insolubility and infusibility, and is used as a flame retardant additive to finish textiles so as to prepare the textiles with better flame retardant property.
Disclosure of Invention
The invention aims to solve the technical problem of providing a graphene aerogel modified flame-retardant fabric based on a microbubble template sol-gel method and a preparation method thereof.
In order to solve the technical problems, the technical scheme of the invention is as follows:
a preparation method of a graphene aerogel modified flame-retardant fabric based on a microbubble template sol-gel method comprises the following steps:
(1) adding alkyl polyglycoside and lauryl sodium sulfate into deionized water, and uniformly dispersing to obtain a foam precursor solution;
(2) adding the graphene oxide solution into DL-cysteine, and preheating and stirring to obtain pre-reduced graphene oxide hydrosol;
(3) mixing the foam precursor solution prepared in the step (1) with the pre-reduced graphene oxide hydrosol prepared in the step (2), placing the fabric in the mixture, shearing at a high speed to form stable foam on the surface of the fabric, taking out the fabric, quickly freezing, and cracking a foam film to prepare and obtain a partially-reduced graphene oxide liquid crystal porous material;
(4) and (4) unfreezing the partially reduced graphene oxide liquid crystal porous material prepared in the step (3) at room temperature, heating to reduce, and then freeze-drying to obtain the graphene aerogel modified flame-retardant fabric.
Preferably, in the step (1), the content of the alkyl polyglycoside in the foam precursor solution is 0.3-0.4%, and the content of the sodium dodecyl sulfate is 0.1-0.15%.
Preferably, in the step (2), the preheating and stirring temperature is 50-60 ℃, the stirring speed is 600-.
Preferably, in the step (2), the dosage ratio of the graphene oxide to the DL-cysteine is 1:5-8, and the content of the graphene oxide is 1-2.5 mg/mL.
Preferably, in the step (3), the rotation speed of the high-speed shearing is 15000-.
As the optimization of the technical proposal, in the step (3), the height of the foam is 80-100 μm, and the density is 500-850/cm 2.
Preferably, in the step (3), the temperature of the rapid freezing is-10 to-20 ℃ and the time is 2 to 4 hours.
Preferably, in the step (3), the size of the partially reduced graphene oxide liquid crystal porous material is 80-100cm, the thickness is 8-15mm, the pore diameter is 84-110 μm, and the wall thickness of the porous material is 3-10 μm.
Preferably, in the step (4), the temperature for the temperature-rising reduction is 70-80 ℃ and the time is 1-2 h.
The invention also provides the graphene aerogel modified flame-retardant fabric based on the microbubble template sol-gel method.
Compared with the prior art, the invention has the following beneficial effects:
(1) the graphene aerogel in the graphene aerogel modified flame-retardant fabric prepared by the invention is deep into the fabric, and a large-size, uniform and complete graphene aerogel structure is formed on the surface of the fabric, the graphene aerogel structure prepared by the invention is combined with a template sol-gel method by adopting a distributed reduction method, the prepared graphene aerogel is regular in structure and good in elasticity, can be compressed by 70-80% and rebounded, and the usable range and the comfort performance of the fabric are improved.
(2) The graphene aerogel in the prepared graphene aerogel modified flame-retardant fabric adopts microbubbles as a template, the graphene oxide spontaneously forms a microcrystalline structure on the surface of the microbubbles by utilizing the characteristic of regular structure of the graphene oxide under the micro-size, the microcrystalline structure of the graphene oxide is stored by means of a quick freezing technology, a large-size, uniform and complete graphene aerogel structure is formed on the surface of the fabric, the graphene aerogel and the fabric are perfectly combined, and the prepared flame-retardant fabric is light in specific gravity, difficult to dissolve and melt, excellent in flame-retardant performance and capable of keeping certain elasticity.
(3) The graphene aerogel with a large size, a uniform and complete structure in the prepared graphene aerogel modified flame-retardant fabric adopts microbubbles with a stable structure and a long half-life period as templates, the alkyl polyglycoside is a nonionic surfactant synthesized from renewable plant raw materials such as fatty alcohol, glucose and the like, the alkyl polyglycoside and the sodium dodecyl sulfate are compounded to prepare a solution with good foaming performance and spreading performance, and the prepared foam material is non-toxic, non-irritant, easily biodegradable, free of influence on the structure and performance of subsequent fabrics, and good in stability and safety.
(4) The preparation method is simple, has strong controllability and low requirement on equipment by simple dipping and stirring processes and freeze drying processes, and is suitable for industrial large-scale production.
Detailed Description
The present invention will be described in detail with reference to specific embodiments, which are illustrative of the invention and are not to be construed as limiting the invention.
Example 1:
(1) adding alkyl polyglycoside and sodium dodecyl sulfate into deionized water, and uniformly dispersing to obtain a foam precursor solution, wherein the content of the alkyl polyglycoside in the foam precursor solution is 0.3%, and the content of the sodium dodecyl sulfate in the foam precursor solution is 0.1%.
(2) Adding 1mg/mL graphene oxide solution into DL-cysteine according to the dosage ratio of the graphene oxide to the DL-cysteine of 1:5, and preheating and stirring at the rotating speed of 600r/min for 15min at 50 ℃ to obtain the pre-reduced graphene oxide hydrosol.
(3) Mixing the foam precursor solution and the pre-reduced graphene oxide hydrosol, placing the fabric in the mixture, shearing the fabric at a high speed of 15000r/min for 30min to form stable foam on the surface of the fabric, wherein the height of the foam is 80-100 mu m, the density is 500/cm 2, taking out the fabric, quickly freezing the fabric at-10 ℃ for 2h, and cracking the foam membrane to prepare the partially reduced graphene oxide liquid crystal porous material, wherein the size of the partially reduced graphene oxide liquid crystal porous material is 80-100cm, the thickness of the partially reduced graphene oxide liquid crystal porous material is 8mm, the pore diameter of the partially reduced graphene oxide liquid crystal porous material is 84-110 mu m, and the wall thickness of the porous material is 3 mu m.
(4) And unfreezing the partially reduced graphene oxide liquid crystal porous material at room temperature, heating to reduce for 1h at 70 ℃, and freeze-drying to obtain the graphene aerogel modified flame-retardant fabric.
Example 2:
(1) adding alkyl polyglycoside and sodium dodecyl sulfate into deionized water, and uniformly dispersing to obtain a foam precursor solution, wherein the content of the alkyl polyglycoside in the foam precursor solution is 0.4%, and the content of the sodium dodecyl sulfate in the foam precursor solution is 0.15%.
(2) Adding 2.5mg/mL of graphene oxide solution into DL-cysteine according to the dosage ratio of the graphene oxide to the DL-cysteine of 1:8, and preheating and stirring at the rotating speed of 2500r/min for 30min at the temperature of 60 ℃ to obtain the pre-reduced graphene oxide hydrosol.
(3) Mixing the foam precursor solution and the pre-reduced graphene oxide hydrosol, placing the fabric in the mixture, shearing the fabric at a high speed of 20000r/min for 60min to form stable foam on the surface of the fabric, wherein the height of the foam is 80-100 mu m, the density is 850/cm 2, taking out the fabric, quickly freezing the fabric at-20 ℃ for 4h, and cracking the foam membrane to prepare the partially reduced graphene oxide liquid crystal porous material, wherein the size of the partially reduced graphene oxide liquid crystal porous material is 80-100cm, the thickness of the partially reduced graphene oxide liquid crystal porous material is 15mm, the pore diameter of the partially reduced graphene oxide liquid crystal porous material is 84-110 mu m, and the wall thickness of the porous material is 10 mu m.
(4) And unfreezing the partially reduced graphene oxide liquid crystal porous material at room temperature, heating to reduce for 2 hours at 80 ℃, and freeze-drying to obtain the graphene aerogel modified flame-retardant fabric.
Example 3:
(1) adding alkyl polyglycoside and sodium dodecyl sulfate into deionized water, and uniformly dispersing to obtain a foam precursor solution, wherein the content of the alkyl polyglycoside in the foam precursor solution is 0.35%, and the content of the sodium dodecyl sulfate in the foam precursor solution is 0.12%.
(2) Adding 1.5mg/mL graphene oxide solution into DL-cysteine according to the dosage ratio of the graphene oxide to the DL-cysteine of 1:6, and preheating and stirring at 53 ℃ at the rotating speed of 1200r/min for 20min to obtain the pre-reduced graphene oxide hydrosol.
(3) Mixing the foam precursor solution and the pre-reduced graphene oxide hydrosol, placing the fabric in the mixture, shearing the fabric at a high speed of 18000r/min for 45min to form stable foam on the surface of the fabric, wherein the height of the foam is 80-100 mu m, the density is 650/cm 2, taking out the fabric, quickly freezing the fabric at-15 ℃ for 3h, and cracking the foam membrane to prepare the partially reduced graphene oxide liquid crystal porous material, wherein the size of the partially reduced graphene oxide liquid crystal porous material is 80-100cm, the thickness of the partially reduced graphene oxide liquid crystal porous material is 12mm, the pore diameter of the partially reduced graphene oxide liquid crystal porous material is 84-110 mu m, and the wall thickness of the porous material is 5 mu m.
(4) And unfreezing the partially reduced graphene oxide liquid crystal porous material at room temperature, heating to reduce for 1.5h at 75 ℃, and freeze-drying to obtain the graphene aerogel modified flame-retardant fabric.
Example 4:
(1) adding alkyl polyglycoside and sodium dodecyl sulfate into deionized water, and uniformly dispersing to obtain a foam precursor solution, wherein the content of the alkyl polyglycoside in the foam precursor solution is 0.37%, and the content of the sodium dodecyl sulfate in the foam precursor solution is 0.14%.
(2) Adding 2.1mg/mL of graphene oxide solution into DL-cysteine according to the dosage ratio of the graphene oxide to the DL-cysteine of 1:7.2, and preheating and stirring at 57 ℃ at the rotating speed of 2300r/min for 20min to obtain the pre-reduced graphene oxide hydrosol.
(3) Mixing the foam precursor solution and the pre-reduced graphene oxide hydrosol, placing the fabric in the mixture, shearing the fabric at a high speed of 19000r/min for 55min to form stable foam on the surface of the fabric, wherein the height of the foam is 80-100 mu m, the density is 700/cm 2, taking out the fabric, quickly freezing the fabric at-15 ℃ for 2.5h, and cracking a foam film to prepare the partially reduced graphene oxide liquid crystal porous material, wherein the size of the partially reduced graphene oxide liquid crystal porous material is 80-100cm, the thickness of the partially reduced graphene oxide liquid crystal porous material is 12mm, the pore diameter of the partially reduced graphene oxide liquid crystal porous material is 84-110 mu m, and the wall thickness of the porous material is 7 mu m.
(4) And unfreezing the partially reduced graphene oxide liquid crystal porous material at room temperature, heating to reduce at 77 ℃ for 1.5h, and freeze-drying to obtain the graphene aerogel modified flame-retardant fabric.
Example 5:
(1) adding alkyl polyglycoside and sodium dodecyl sulfate into deionized water, and uniformly dispersing to obtain a foam precursor solution, wherein the content of the alkyl polyglycoside in the foam precursor solution is 0.39%, and the content of the sodium dodecyl sulfate in the foam precursor solution is 0.11%.
(2) Adding 1.8mg/mL graphene oxide solution into DL-cysteine according to the dosage ratio of the graphene oxide to the DL-cysteine of 1:6, and preheating and stirring at the rotating speed of 2400r/min for 20min at the temperature of 59 ℃ to obtain the pre-reduced graphene oxide hydrosol.
(3) Mixing the foam precursor solution and the pre-reduced graphene oxide hydrosol, placing the fabric in the mixture, shearing the fabric at a high speed of 18500r/min for 40min to form stable foam on the surface of the fabric, wherein the height of the foam is 80-100 mu m, the density is 710/cm 2, taking out the fabric, quickly freezing the fabric at-17 ℃ for 3.5h, and cracking a foam film to prepare the partially reduced graphene oxide liquid crystal porous material, wherein the size of the partially reduced graphene oxide liquid crystal porous material is 80-100cm, the thickness of the partially reduced graphene oxide liquid crystal porous material is 10mm, the pore diameter of the partially reduced graphene oxide liquid crystal porous material is 84-110 mu m, and the wall thickness of the porous material is 4 mu m.
(4) And unfreezing the partially reduced graphene oxide liquid crystal porous material at room temperature, heating to reduce for 2 hours at 75 ℃, and freeze-drying to obtain the graphene aerogel modified flame-retardant fabric.
Example 6:
(1) adding alkyl polyglycoside and sodium dodecyl sulfate into deionized water, and uniformly dispersing to obtain a foam precursor solution, wherein the content of the alkyl polyglycoside in the foam precursor solution is 0.3%, and the content of the sodium dodecyl sulfate in the foam precursor solution is 0.15%.
(2) Adding 2.5mg/mL graphene oxide solution into DL-cysteine according to the dosage ratio of the graphene oxide to the DL-cysteine of 1:5, and preheating and stirring at the rotating speed of 2500r/min for 15min at 50 ℃ to obtain the pre-reduced graphene oxide hydrosol.
(3) Mixing the foam precursor solution and the pre-reduced graphene oxide hydrosol, placing the fabric in the mixture, shearing the fabric at a high speed of 20000r/min for 30min to form stable foam on the surface of the fabric, wherein the height of the foam is 80-100 mu m, the density is 850/cm 2, taking out the fabric, quickly freezing the fabric at-10 ℃ for 4h, and cracking the foam membrane to prepare the partially reduced graphene oxide liquid crystal porous material, wherein the size of the partially reduced graphene oxide liquid crystal porous material is 80-100cm, the thickness of the partially reduced graphene oxide liquid crystal porous material is 8mm, the pore diameter of the partially reduced graphene oxide liquid crystal porous material is 84-110 mu m, and the wall thickness of the porous material is 10 mu m.
(4) And unfreezing the partially reduced graphene oxide liquid crystal porous material at room temperature, heating to reduce for 2 hours at 70 ℃, and freeze-drying to obtain the graphene aerogel modified flame-retardant fabric.
The results of testing the resilience, flame retardancy and mechanical properties of the graphene aerogel modified flame retardant fabrics prepared in examples 1 to 6 and the untreated fabric are as follows:
as can be seen from the above table, the graphene aerogel modified flame-retardant fabric prepared by the method disclosed by the invention is good in flexibility, excellent in flame retardant property and remarkably improved in mechanical property.
The foregoing embodiments are merely illustrative of the principles and utilities of the present invention and are not intended to limit the invention. Any person skilled in the art can modify or change the above-mentioned embodiments without departing from the spirit and scope of the present invention. Accordingly, it is intended that all equivalent modifications or changes which can be made by those skilled in the art without departing from the spirit and technical spirit of the present invention be covered by the claims of the present invention.
Claims (9)
1. A preparation method of a graphene aerogel modified flame-retardant fabric based on a microbubble template sol-gel method is characterized by comprising the following steps:
(1) adding alkyl polyglycoside and lauryl sodium sulfate into deionized water, and uniformly dispersing to obtain a foam precursor solution; the content of alkyl polyglycoside in the foam precursor solution is 0.3-0.4%, and the content of sodium dodecyl sulfate is 0.1-0.15%;
(2) adding the graphene oxide solution into DL-cysteine, and preheating and stirring to obtain pre-reduced graphene oxide hydrosol;
(3) mixing the foam precursor solution prepared in the step (1) with the pre-reduced graphene oxide hydrosol prepared in the step (2), placing the fabric in the mixture, shearing at a high speed to form stable foam on the surface of the fabric, taking out the fabric, quickly freezing, and cracking a foam film to prepare and obtain a partially-reduced graphene oxide liquid crystal porous material;
(4) and (4) unfreezing the partially reduced graphene oxide liquid crystal porous material prepared in the step (3) at room temperature, heating to reduce, and then freeze-drying to obtain the graphene aerogel modified flame-retardant fabric.
2. The preparation method of the graphene aerogel modified flame-retardant fabric based on the microbubble template sol-gel method according to claim 1, characterized in that: in the step (2), the preheating and stirring temperature is 50-60 ℃, the stirring speed is 600-2500r/min, and the time is 15-30 min.
3. The preparation method of the graphene aerogel modified flame-retardant fabric based on the microbubble template sol-gel method according to claim 1, characterized in that: in the step (2), the dosage ratio of the graphene oxide to the DL-cysteine is 1:5-8, and the content of the graphene oxide is 1-2.5 mg/mL.
4. The preparation method of the graphene aerogel modified flame-retardant fabric based on the microbubble template sol-gel method according to claim 1, characterized in that: in the step (3), the rotation speed of the high-speed shearing is 15000-.
5. The preparation method of the graphene aerogel modified flame-retardant fabric based on the microbubble template sol-gel method according to claim 1, characterized in that: in the step (3), the height of the foam is80-100 μm, density of 500-2。
6. The preparation method of the graphene aerogel modified flame-retardant fabric based on the microbubble template sol-gel method according to claim 1, characterized in that: in the step (3), the temperature of quick freezing is-10 to-20 ℃, and the time is 2 to 4 hours.
7. The preparation method of the graphene aerogel modified flame-retardant fabric based on the microbubble template sol-gel method according to claim 1, characterized in that: in the step (3), the size of the partially reduced graphene oxide liquid crystal porous material is 80-100cm, the thickness is 8-15mm, the pore diameter is 84-110 μm, and the wall thickness of the porous material is 3-10 μm.
8. The preparation method of the graphene aerogel modified flame-retardant fabric based on the microbubble template sol-gel method according to claim 1, characterized in that: in the step (4), the temperature for heating reduction is 70-80 ℃ and the time is 1-2 h.
9. A graphene aerogel modified flame-retardant fabric prepared by the preparation method of any one of claims 1 to 8 based on a micro-bubble template sol-gel method.
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