CN112359597B - Organic/inorganic hybrid film-coated cotton textile and preparation method thereof - Google Patents
Organic/inorganic hybrid film-coated cotton textile and preparation method thereof Download PDFInfo
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Abstract
本发明涉及一种有机/无机杂化薄膜包覆棉纺织品及其制备方法，首先向棉纺织品表面依次均匀喷涂含磷酸基团的离子型助剂、过渡金属的可溶盐溶液、含有‑NH‑基团的离子型助剂以及海泡石分散液，然后对喷涂后的棉纺织品进行烘干，最后多次重复上述步骤制得有机/无机杂化薄膜包覆棉纺织品；制得的有机/无机杂化薄膜包覆棉纺织品中有机/无机杂化薄膜包括含磷酸基团的离子型助剂、过渡金属离子、含有‑NH‑基团的离子型助剂和纳米海泡石；离子型助剂与棉纺织品之间以及离子型助剂与纳米海泡石之间通过过渡金属离子的离子键及配位键相结合。本发明的方法简单易行；制得的有机/无机杂化薄膜包覆棉纺织品手感比较好，力学性能增强，阻燃性能大幅度提升。
The invention relates to an organic/inorganic hybrid film-coated cotton textile and a preparation method thereof. First, the surface of the cotton textile is uniformly sprayed with an ionic auxiliary agent containing a phosphoric acid group, a soluble salt solution of a transition metal, and a -NH- group of ionic auxiliaries and sepiolite dispersion, then drying the sprayed cotton textiles, and finally repeating the above steps for many times to obtain organic/inorganic hybrid film-coated cotton textiles; the prepared organic/inorganic Organic/inorganic hybrid films in hybrid film-covered cotton textiles include ionic auxiliaries containing phosphoric acid groups, transition metal ions, ionic auxiliaries containing ‑NH‑ groups and nano-sepiolite; ionic auxiliaries It is combined with cotton textiles and between ionic auxiliaries and nano-sepiolite through ionic bonds and coordination bonds of transition metal ions. The method of the invention is simple and easy to implement; the prepared organic/inorganic hybrid film-coated cotton textile has better hand feeling, enhanced mechanical properties and greatly improved flame retardant properties.
Description
Technical Field
The invention belongs to the technical field of textile finishing and processing, and relates to an organic/inorganic hybrid film-coated cotton textile and a preparation method thereof.
Background
With the development of society and economy, the status of various textiles in human life is more and more important, and the application range is wider, however, most of the textiles belong to flammable materials and are direct causes of most of fires, especially cotton textiles. Therefore, how to prevent the harm caused by textile burning and reduce the loss of people's life and economy has attracted attention of all the world.
The flame retardance of textile materials began in 1820, and Gay-lussac found for the first time that the mixture of amine salt and borax can be used for flame retardance of fibers, which opened up the way for flame retardance research. Flame retardants for textiles can be classified into temporary flame retardants, semi-durable flame retardants, and durable flame retardants according to their flame retardant effects. The finishing method mainly comprises the following steps: sol-gel method, padding baking method, coating method, layer-by-layer assembling method, dual curing method, microcapsule preparation method, plasma method and flame-retardant fiber spinning method. However, the traditional flame-retardant textile finishing has the defects of standard formaldehyde release, non-durable flame-retardant effect, rough and hard hand feeling and the like, and limits the application field of the flame-retardant finished textile material.
Disclosure of Invention
The present invention is directed to solving the above problems of the prior art and to providing an organic/inorganic hybrid film-coated cotton textile and a method for preparing the same.
In order to achieve the purpose, the technical scheme adopted by the invention is as follows:
a preparation method of organic/inorganic hybrid film coated cotton textile adopts a method of combining a spraying method and a Layer-by-Layer self-assembly method (Layer-by-Layer), and comprises the following steps:
(1) firstly, uniformly spraying a solution of an ionic assistant containing a phosphoric acid group on the surface of a cotton textile in sequence (the molecular structure of the ionic assistant containing the phosphoric acid group contains a large number of-P ═ O and-O-groups, and the outermost layer of an oxygen atom in the structure has lone pair electrons, has stronger electron donating capability and can form stronger coordination action with transition metal ions), a soluble salt solution of transition metal, a solution of the ionic assistant containing-NH-groups and a sepiolite dispersion solution;
(2) then drying the sprayed cotton textile;
(3) and finally, repeating the steps (1) to (2) for multiple times to obtain the organic/inorganic hybrid film-coated cotton textile.
As a preferred technical scheme:
the solution of the ionic auxiliary agent containing the phosphoric acid group is water-soluble phytate solution, the solution of the ionic auxiliary agent containing the-NH-group is water-soluble polyaspartate solution, the water-soluble polyaspartate contains-OH, -C ═ O and-O-groups besides the-NH-group, the outermost layer of the oxygen atom in the structure has lone pair electrons, has stronger electron donating capability and can form stronger coordination action with transition metal ions, and the ionic auxiliary agent containing the-NH-group can also be diethylenetriamine solution or ethylene diamine tetraacetic acid disodium salt solution and the like.
According to the preparation method of the organic/inorganic hybrid film-coated cotton textile, the concentration of the sepiolite dispersion liquid is 3-10 g/L; the sepiolite dispersion liquid is obtained by dispersing nano sepiolite in deionized water and stirring; the dispersion liquid can not be layered after standing for more than 72 hours, and the full dispersion and dissociation of the nano sepiolite are ensured;
the water-soluble phytate solution is obtained by dissolving phytate in deionized water and stirring, and the concentration of the water-soluble phytate solution is 5-52 g/L;
the water-soluble polyaspartic acid salt solution is obtained by dissolving sodium polyaspartate in deionized water and stirring, and the concentration of the water-soluble polyaspartic acid salt solution is 5-21 g/L;
the soluble salt solution of the transition metal is obtained by dissolving the soluble salt of the transition metal in deionized water and stirring, and the concentration of the soluble salt solution of the transition metal is 2-22 g/L.
In the preparation method of the organic/inorganic hybrid film-coated cotton textile, the water-soluble phytate is sodium phytate or potassium phytate;
the water-soluble polyaspartate is sodium polyaspartate or potassium polyaspartate;
the transition metal is iron, zinc, copper, nickel, titanium or vanadium.
The preparation method of the organic/inorganic hybrid film-coated cotton textile comprises the following specific steps of (1): firstly, respectively filling a solution of an ionic auxiliary agent containing a phosphoric acid group, a soluble salt solution of transition metal, a solution of an ionic auxiliary agent containing an-NH-group and a sepiolite dispersion liquid into different spray pots, adjusting the spraying effect of the spray pots to be mist, then spraying the solution of the ionic auxiliary agent containing the phosphoric acid group on a pure cotton fabric fixed on a cloth stretching frame as a base material, then spraying the solution of the ionic auxiliary agent containing the phosphoric acid group, then spraying the solution of the ionic auxiliary agent containing the-NH-group, then placing the mixture into an oven to be dried for 3-5 min to be semi-dried at 90 ℃, then spraying the sepiolite dispersion liquid, and finally continuing placing the mixture into the oven to be dried for 3-5 min to be semi-dried at 90 ℃;
the mass ratio of the solute in the solution of the phosphate group-containing ionic auxiliary sprayed in the step (1), the solute in the solution of the-NH-group-containing ionic auxiliary, the solute in the soluble salt solution of the transition metal and the dispersoid in the sepiolite dispersion liquid is 30-60: 3-6: 15-25: 8-15;
and (2) spraying a solution of the ionic assistant containing the phosphoric acid group, a solution of the ionic assistant containing the-NH-group, a soluble salt solution of the transition metal and a sepiolite dispersion liquid in the step (1) to form a film, wherein the thickness of the formed film is 50-150 nm.
According to the preparation method of the organic/inorganic hybrid film-coated cotton textile, the drying temperature in the step (2) is 90-110 ℃, and the time is 5-10 min.
According to the preparation method of the organic/inorganic hybrid film-coated cotton textile, the number of times of repeating the steps (1) to (2) in the step (3) is 5-20; if the times are too few, the flame retardant effect is not achieved, if the times are too many, the hand feeling is influenced, and the fastness of the hybrid film coated cotton fabric is also reduced.
The invention also provides the cotton textile coated with the organic/inorganic hybrid film prepared by the method, wherein the surface of the cotton textile is coated with a plurality of layers of organic/inorganic hybrid films, and each layer of organic/inorganic hybrid film comprises an ionic auxiliary agent containing phosphate groups, transition metal ions, an ionic auxiliary agent containing-NH-groups and nano-sepiolite;
in the organic/inorganic hybrid film adhered to the surface of the cotton textile, the ionic auxiliary agent containing the phosphoric acid group is combined with the nano-sepiolite, the ionic auxiliary agent containing the-NH-group is combined with the cotton textile, and the ionic auxiliary agent containing the-NH-group is combined with the nano-sepiolite through ionic bonds and coordinate bonds of transition metal ions, in short, the transition metal ions are used as a connecting agent to combine all the components together.
As a preferred technical scheme:
the organic/inorganic hybrid film-coated cotton textile can achieve the V0 flame retardance of the flame retardance standard UL 94; the afterflame time is 0-10 s, the smoldering time is 0-19 s, and the LOI is 19-28%.
The warp-direction breaking strength and the weft-direction breaking strength of the organic/inorganic hybrid film coated cotton textile are 720-860N and 307-420N respectively, and the warp-direction breaking elongation and the weft-direction breaking elongation are 14-20% and 14-18% respectively (the breaking strength and the breaking elongation of the cotton fabric are tested according to the national standard GB3923.1-2013, and the test result shows that the breaking strength is slightly higher than that of a pure cotton fabric, which indicates that the strength of the material is improved after the organic/inorganic hybrid film is coated, and the index of a clothing product can be met).
The principle of the invention is as follows:
the traditional method mainly adopts a combination of a Layer-by-Layer method and an impregnation method, substances with different charges are coated on the surface of a base material, component assembly reactions with different properties occur in the impregnation process, the reaction time is short, the reaction is incomplete, the coating of the base material is not perfect by adopting the film prepared by the method, the base material is repeatedly impregnated in solutions with different components, the concentration fluctuation of the solution is caused, the film thickness of the film and the coating effect on the base material are influenced, and the other defect of the repeated impregnation is that the coating of the coated film falls off in the impregnation process, and the coating effect is poor;
the invention combines the Layer-by-Layer with the spraying method, the components with different properties are coated on the surface of the base material, the spraying effect of the spray gun is adjusted to be in a spraying shape during spraying, a uniform liquid film can be formed on the surface of the base material, a micro-solution system is constructed, the substances with different properties are assembled in the micro-solution system, the components can be continuously assembled in the drying process after spraying, about 5 minutes is probably, the assembly of the traditional Layer-by-Layer method is that the base material is assembled in a few seconds of solution dipping, compared with the traditional method which combines the Layer-by-Layer with the dipping method, the assembly time of the invention is longer, the different components can fully react, and the fastness of the finally coated hybrid film is better; the concentration of each component is stable, the spraying times are controlled, the quantity of chemical substances contained in each Layer of film constructed by the Layer-by-Layer method is balanced, the stability of the thickness of the film is ensured, and the coating effect of the film on a base material is good.
The traditional flame-retardant after-finishing of textiles has the defects of overproof formaldehyde release, non-durable flame-retardant effect, rough hand feeling and the like.
The organic/inorganic hybrid film is constructed by taking cotton textiles as a base material, and constructing a plurality of layers of organic/inorganic hybrid films on the surface of the base material by using nano sepiolite, chelating aids (ionic aids containing phosphoric acid groups and ionic aids containing-NH-groups) and transition metal ions through a spraying method and a layer-by-layer self-assembly method. As the surface of the cotton textile contains rich-OH, a large amount of Si-OH also exists on the surface of the nano sepiolite, and the cotton textile and the nano sepiolite can be connected by transition metal ions theoretically. However, the cotton cellulose molecules in the cotton textiles have larger volume and larger steric hindrance, and the nano sepiolite also has larger steric hindrance. Therefore, the invention adopts a chelating auxiliary agent containing phosphorus and nitrogen as a connecting agent, because a large amount of-OH, -C ═ O, -P ═ O, -O-groups, especially-C ═ O and-P ═ O groups exist in the molecular structure of the chelating auxiliary agent (because the electrons of the oxygen atom in the double bond are delocalized and the electrons of the single bond oxygen are localized, the electronegativity of the double bond oxygen is stronger, and the coordination bond is easier to form), the lone pair electrons exist in the outermost layer of the oxygen atoms in the two structures, and the nano sepiolite has stronger electron donating capability, can form stronger coordination action with the transition metal ions, and simultaneously, the transition metal ions can also form a chemical action with-OH on the surface of the cotton fibers, Si-OH on the surface of the nano sepiolite is combined by ionic bonds. Therefore, the addition of the chelating agent can enhance the binding capacity of the sepiolite and the cotton fabric, namely enhance the durability of the sepiolite-coated cotton fabric, so that an organic/inorganic hybrid film with high fastness is formed on the surface of the cotton fabric.
The traditional durable flame-retardant finishing mainly adopts a baking method, flame retardants containing phosphorus and nitrogen elements are grafted on the surface of cotton fibers, Pyrovatex CP series flame retardants and-OH in a cotton fiber structure are subjected to chemical reaction in the reaction process to generate covalent bonds for combination, and formaldehyde is released in the reaction process.
The method for coating the cotton textile by the organic/inorganic hybrid film endows the material with durable flame retardance, the surface of the cotton textile is still coated by the hybrid film after washing, and the flame retardance test verifies that the material after washing has flame retardance, which shows that the flame-retardant finishing method disclosed by the invention has durability.
According to the invention, the organic/inorganic hybrid film is constructed on the surface of the cotton fabric by adopting the phytic acid, the transition metal ions, the polyaspartic acid and the nano sepiolite, and the sepiolite has certain flexibility, so that the nano sepiolite is compact in coating on the cotton fiber, the cotton fabric coated by the hybrid film is soft in handfeel, and the defect that the fabric is hard after traditional flame-retardant finishing is overcome.
Has the advantages that:
(1) the invention combines a spraying method and a layer-by-layer self-assembly method, firstly coats the phytate radical, the iron ion, the polyaspartic acid ion and the nano sepiolite on the surface of the cotton fabric through chemical action to form an organic/inorganic hybrid film, and firstly applies the hybrid film to the field of flame retardance of the cotton fabric;
(2) the method is very convenient and fast, and can be used for industrial production;
(3) the organic/inorganic hybrid film-coated cotton textile prepared by the method has good hand feeling, enhanced mechanical property and greatly improved flame retardant property.
Drawings
FIG. 1 is an SEM image of an organic/inorganic hybrid film coated cotton fabric of the present invention, wherein the magnification of the image a is 5000, the magnification of the image b is 2000, and the magnification of the image c is 200;
FIG. 2 is a structural mechanism diagram of an organic/inorganic hybrid film on the surface of a cotton textile, wherein 1BL represents each unit layer of the organic/inorganic hybrid film;
FIG. 3 is a flow chart of the construction of an organic/inorganic hybrid film on the surface of a cotton textile, in which,
is a starting position;
fig. 4 is a photograph of a vertical burn of a sample, wherein a. pure cotton; b. before the hybrid film is coated with cotton and washed with water; c. coating the hybrid film with cotton, and washing; d. coating cotton with sepiolite before water washing; e. coating the sepiolite with cotton, and washing with water;
fig. 5 is a TEM image of stripped sepiolite.
Detailed Description
The invention will be further illustrated with reference to specific embodiments. It should be understood that these examples are for illustrative purposes only and are not intended to limit the scope of the present invention. Further, it should be understood that various changes or modifications of the present invention may be made by those skilled in the art after reading the teaching of the present invention, and such equivalents may fall within the scope of the present invention as defined in the appended claims.
Example 1
A preparation method of an organic/inorganic hybrid membrane-coated cotton textile comprises the following steps:
(1) firstly, uniformly spraying a sodium phytate solution (the concentration is 5g/L), a ferric nitrate nonahydrate solution (the concentration is 2g/L), a sodium polyaspartate solution (the concentration is 5g/L, and the molecular weight of the sodium polyaspartate is M.W-7000) and a nano sepiolite dispersion solution (the concentration is 3g/L) on the surface of a cotton textile in sequence; as shown in fig. 5, the specific dimensions of the nano sepiolite are: length of nano sepiolite: 10 μm, width: 10 nm;
the specific spraying process is shown in fig. 3: firstly, respectively filling a sodium phytate solution, a ferric nitrate nonahydrate solution, a sodium polyaspartate solution and a nano sepiolite dispersion liquid into different spray pots, adjusting the spraying effect of the spray pots to be mist, then spraying the sodium phytate solution, then spraying the ferric nitrate nonahydrate solution, then spraying the sodium polyaspartate solution, then placing the sodium polyaspartate solution into a drying oven to be dried for 3min at 90 ℃, then spraying the nano sepiolite dispersion liquid, and finally continuously placing the drying oven into the drying oven to be dried for 3min at 90 ℃;
the mass ratio of the solute in the sprayed sodium phytate solution, the solute in the sodium polyaspartate solution, the solute in the ferric nitrate nonahydrate solution and the dispersoid in the nano sepiolite dispersion liquid is 30:3:15: 8; the thickness of a film formed after spraying the sodium phytate solution, the sodium polyaspartate solution, the ferric nitrate nonahydrate solution and the nano sepiolite dispersion liquid is 50 nm;
(2) then drying the sprayed cotton textile at 90 ℃ for 5 min;
(3) and (3) finally, repeating the processes of the steps (1) to (2) for 5 times to obtain the organic/inorganic hybrid film-coated cotton textile.
As shown in fig. 1, which is an SEM image of the organic/inorganic hybrid film coated cotton fabric of the present invention, the surface of the fiber is uniformly coated with a uniform and dense film formed of nano sepiolite, wherein, the magnification of the a diagram is 5000, the magnification of the b diagram is 2000, and the magnification of the c diagram is 200; the surface of the cotton textile is coated with a plurality of layers of organic/inorganic hybrid films, and each layer of organic/inorganic hybrid film comprises sodium phytate, ferric iron ions, sodium polyaspartate and nano sepiolite; in the organic/inorganic hybrid film attached to the surface of the cotton textile, sodium phytate is combined with nano sepiolite, sodium polyaspartate is combined with the cotton textile, and sodium polyaspartate is combined with nano sepiolite through ionic bonds and coordination bonds of ferric ions. As shown in FIG. 2, which is a structural mechanism diagram of the organic/inorganic hybrid film on the surface of the cotton textile, since the surface of the cotton textile contains abundant-OH, the surface of the nano-sepiolite also contains a large amount of Si-OH, the two can be linked by a transition metal ion theoretically. However, the cotton cellulose molecules in the cotton textiles have larger volume and larger steric hindrance, and the nano sepiolite also has larger steric hindrance. Therefore, the nano sepiolite is coated on the surface of the cotton fabric by a strong acting force and needs another substance which can generate a chemical action with transition metal ions3+) Forming stronger coordination; meanwhile, the transition metal ions can be combined with-OH on the surface of the cotton fiber and Si-OH on the surface of the nano sepiolite by ionic bonds.
Comparative example 1
The preparation method of the organic/inorganic hybrid membrane-coated cotton textile is basically the same as that in the example 1, except that only nano sepiolite dispersion liquid (the concentration is 3g/L) is uniformly sprayed on the surface of the cotton textile in the step (1), and the thickness of a formed membrane is equal to that of the formed membrane after spraying the sodium phytate solution, the sodium polyaspartate solution, the ferric nitrate nonahydrate solution and the nano sepiolite dispersion liquid in the example 1.
The pure cotton was designated sample a, the product prepared in example 1 was designated sample b, and the product prepared in comparative example 1 was designated sample d; soaping and drying the sample d and the sample b according to the national standard GB/T3921.1-1997 textile color fastness test to obtain a sample e and a sample c respectively; the flame retardant performance of the samples a, b, c, d and e was analyzed by a vertical combustion tester (YBG168, Ningbo textile Instrument Co., Ltd.), the data is shown in Table 1, and the photo of the sample after the test is shown in FIG. 4; performing an oxygen limiting index test on the cotton fabric by using a limiting oxygen index tester (LOI, 5801A-01, Suzhou Yinhui detection technology Co., Ltd.), wherein the data are shown in Table 1; an electronic universal tester (WDW-50, Shanghaineton instruments manufacturing Co., Ltd.) is adopted to carry out tensile property test on the cotton fabric, and the data are shown in Table 2;
TABLE 1 sample flame retardancy test data
Table 2 sample mechanical property test data
As can be seen from the flame retardant test data of the samples in FIG. 4 and Table 1, the afterflame time and the smoldering time of the cotton fabric coated by the organic/inorganic hybrid membrane are greatly reduced, the limited oxygen index is increased by 17-44%, and the burning carbon length of the cotton fabric after flame retardant treatment is reduced (as can be seen from FIG. 4), so that the cotton fabric has self-extinguishing property. The data show that the flame retardant property of the cotton fabric is greatly improved after the flame retardant treatment, and the cotton fabric still has certain flame retardant property after washing. In conclusion, the flame-retardant finishing process can endow the cotton fabric with better durable flame retardance. The conclusion can be drawn from the mechanical property data of the materials in the table 2, the mechanical property of the cotton fabric coated by the organic/inorganic hybrid film is better, and the flame-retardant finishing method is more excellent and is more suitable for large-scale application of the cotton fabric.
Comparative example 2
The preparation method of the organic/inorganic hybrid membrane-coated cotton textile is basically the same as that in the example 1, except that in the step (1), a ferric nitrate nonahydrate solution (with the concentration of 2g/L) and a nano sepiolite dispersion liquid (with the concentration of 3g/L) are uniformly sprayed on the surface of the cotton textile, and the thickness of a formed membrane is the sum of the thickness of the formed membrane after the sodium phytate solution, the sodium polyaspartate solution and the ferric nitrate nonahydrate solution are sprayed and the thickness of the formed membrane after the nano sepiolite dispersion liquid is sprayed.
The finally prepared organic/inorganic hybrid film-coated cotton textile has the afterflame time of 4s, the smoldering time of 16s and the LOI of 22 percent; the breaking strength in the warp direction and that in the weft direction were 791N and 321N, respectively, and the breaking elongation in the warp direction and that in the weft direction were 14% and 16%, respectively.
Compared with example 1, comparative example 2 has longer afterflame time and smoldering time than example 1, has lower strength at break in the warp and weft directions than example 1, and has lower elongation at break in the warp and weft directions than example 1, because the cotton fabric of comparative example 2, although coated with sepiolite fibers and ferric nitrate solution, has inferior flame retardancy to the cotton fabric coated with the organic/inorganic hybrid film of example 1, and thus has longer afterflame time and smoldering time and poorer flame retardancy; the main components of the coating film in the comparative example 2 are sepiolite and iron salt, wherein iron exists in the form of ions, and substances with oxidation, such as oxygen, existing in the environment can cause certain damage to the strength of cotton fabrics under the catalysis of iron; the iron ions in the example 1 are fixed in the hybrid membrane structure by the phosphate groups in the sodium phytate through coordination bonds, so that the strong force of the cotton fabric cannot be damaged, and after the cotton fabric is coated by the sepiolite with the microfiber structure, a layer of organic/inorganic hybrid membrane is formed on the surface of the sepiolite, so that the strong force of the cotton fabric is enhanced.
Example 2
A preparation method of an organic/inorganic hybrid membrane-coated cotton textile comprises the following steps:
(1) firstly, uniformly spraying a sodium phytate solution (the concentration is 10g/L), a ferric nitrate nonahydrate solution (the concentration is 6g/L), a sodium polyaspartate solution (the concentration is 7g/L, the molecular weight is M.W to 7000-8000) and a nano sepiolite dispersion solution (the concentration is 4g/L, the specific size is that the length of the nano sepiolite is 10 mu m, and the width is 10 nm;);
the specific spraying process comprises the following steps: firstly, respectively filling a sodium phytate solution, a ferric nitrate nonahydrate solution, a sodium polyaspartate solution and a nano sepiolite dispersion liquid into different spray pots, adjusting the spraying effect of the spray pots to be mist, then spraying the sodium phytate solution, then spraying the ferric nitrate nonahydrate solution, then spraying the sodium polyaspartate solution, then placing the sodium polyaspartate solution into a drying oven to be dried for 3min at 90 ℃, then spraying the nano sepiolite dispersion liquid, and finally continuously placing the drying oven into the drying oven to be dried for 3min at 90 ℃;
the mass ratio of the solute in the sprayed sodium phytate solution, the solute in the sodium polyaspartate solution, the solute in the ferric nitrate nonahydrate solution and the dispersoid in the nano sepiolite dispersion liquid is 60:3:15: 8; the thickness of a film formed after spraying the sodium phytate solution, the sodium polyaspartate solution, the ferric nitrate nonahydrate solution and the nano sepiolite dispersion liquid is 130 nm;
(2) then drying the sprayed cotton textile at 95 ℃ for 6 min;
(3) and (3) repeating the processes of the steps (1) to (2) for 8 times to obtain the organic/inorganic hybrid film-coated cotton textile.
The finally prepared cotton textile coated with the organic/inorganic hybrid membrane has the surface coated with a plurality of layers of organic/inorganic hybrid membranes, and each layer of organic/inorganic hybrid membrane comprises sodium phytate and transition metal ions (Fe)3+) Sodium polyaspartate and nano sepiolite; in the organic/inorganic hybrid film layer attached to the surface of the cotton textile, sodium phytate is combined with nano sepiolite, sodium polyaspartate is combined with the cotton textile, and sodium polyaspartate is combined with nano sepiolite through ionic bonds and coordination bonds of transition metal ions; the organic/inorganic hybrid film coated cotton textile achieves V0 level flame retardance of flame retardance standard UL94, the afterflame time is 3s, the smoldering time is 10s, and the LOI is 24%; the warp and weft breaking strengths were 810N and 330N, respectively, and the warp and weft elongations at break were 16% and 15%, respectively.
Example 3
A preparation method of an organic/inorganic hybrid membrane-coated cotton textile comprises the following steps:
(1) firstly, uniformly spraying a potassium phytate solution (the concentration is 20g/L), a zinc nitrate hexahydrate solution (the concentration is 10g/L), a sodium polyaspartate solution (the concentration is 12g/L, the molecular weight is M.W to 7000-8000) and a nano sepiolite dispersion solution (the concentration is 5g/L, the specific size is that the length of the nano sepiolite is 20 mu m, the width is 30 nm);
the specific spraying process comprises the following steps: firstly, respectively filling a potassium phytate solution, a zinc nitrate hexahydrate solution, a sodium polyaspartate solution and a nano sepiolite dispersion liquid into different spray pots, adjusting the spraying effect of the spray pots to be mist, then spraying the potassium phytate solution, the zinc nitrate hexahydrate solution, the sodium polyaspartate solution, the drying at 90 ℃ for 4min, the nano sepiolite dispersion liquid and the drying at 90 ℃ for 4min, wherein the pure cotton fabric fixed on a cloth stretching frame is used as a base material;
the mass ratio of the solute in the sprayed potassium phytate solution, the solute in the sodium polyaspartate solution, the solute in the zinc nitrate hexahydrate solution and the dispersoid in the nano sepiolite dispersion liquid is 30:6:15: 8; spraying potassium phytate solution, sodium polyaspartate solution, zinc nitrate hexahydrate solution and nano sepiolite dispersion liquid to form a film with the thickness of 100 nm;
(2) then drying the sprayed cotton textile at 100 ℃ for 6 min;
(3) and (3) repeating the processes of the steps (1) to (2) for 12 times to obtain the organic/inorganic hybrid film-coated cotton textile.
The finally prepared cotton textile coated with the organic/inorganic hybrid membrane has the surface coated with a plurality of layers of organic/inorganic hybrid membranes, and each layer of organic/inorganic hybrid membrane comprises potassium phytate and transition metal ions (Zn)2+) Sodium polyaspartate and nano sepiolite; in the organic/inorganic hybrid film layer attached to the surface of the cotton textile, potassium phytate and nano sepiolite, sodium polyaspartate and the cotton textile, and sodium polyaspartate and nano sepiolite are combined through ionic bonds and coordination bonds of transition metal ions; the organic/inorganic hybrid film coated cotton textile achieves V0 level flame retardance of flame retardance standard UL94, the afterflame time is 3s, the smoldering time is 9s, and the LOI is 24%; the warp and weft breaking strengths were 815N and 336N, respectively, and the warp and weft elongations at break were 16% and 17%, respectively.
Example 4
A preparation method of an organic/inorganic hybrid membrane-coated cotton textile comprises the following steps:
(1) firstly, uniformly spraying a potassium phytate solution (with the concentration of 30g/L), a zinc nitrate hexahydrate solution (with the concentration of 15g/L), a potassium polyaspartate solution (with the concentration of 15g/L and the molecular weight of M.W of 7000-8000) and a nano sepiolite dispersion solution (with the concentration of 6g/L, wherein the specific size is that the length of the nano sepiolite is 20 mu m, and the width of the nano sepiolite is 30 nm);
the specific spraying process comprises the following steps: firstly, respectively filling a potassium phytate solution, a zinc nitrate hexahydrate solution, a potassium polyaspartate solution and a nano sepiolite dispersion liquid into different spray pots, adjusting the spraying effect of the spray pots to be mist, then spraying the potassium phytate solution, the zinc nitrate hexahydrate solution, the potassium polyaspartate solution, the nano sepiolite dispersion liquid and the pure cotton fabric fixed on a cloth stretching frame as a base material, placing the base material in a drying oven to dry for 4min at 90 ℃, then spraying the nano sepiolite dispersion liquid, and finally continuing to place the base material in the drying oven to dry for 4min at 90 ℃;
the mass ratio of the solute in the sprayed potassium phytate solution, the solute in the potassium polyaspartate solution, the solute in the zinc nitrate hexahydrate solution and the dispersoid in the nano sepiolite dispersion liquid is 30:3:15: 8; spraying potassium phytate solution, potassium polyaspartate solution, zinc nitrate hexahydrate solution and nano sepiolite dispersion liquid to form a film with the thickness of 110 nm;
(2) then drying the sprayed cotton textile at the drying temperature of 102 ℃ for 7 min;
(3) and (3) repeating the processes of the steps (1) to (2) for 15 times to obtain the organic/inorganic hybrid film-coated cotton textile.
The finally prepared cotton textile coated with the organic/inorganic hybrid membrane has the surface coated with a plurality of layers of organic/inorganic hybrid membranes, and each layer of organic/inorganic hybrid membrane comprises potassium phytate and transition metal ions (Zn)2+) Potassium polyaspartate and nano sepiolite; in the organic/inorganic hybrid film layer attached to the surface of the cotton textile, potassium phytate and nano sepiolite, potassium polyaspartate and the cotton textile, and potassium polyaspartate and nano sepiolite are combined through ionic bonds and coordination bonds of transition metal ions; the organic/inorganic hybrid film coated cotton textile achieves V0 level flame retardance of flame retardance standard UL94, the afterflame time is 2s, the smoldering time is 7s, and the LOI is 25%; the warp and weft breaking strengths were 830N and 340N, respectively, and the warp and weft elongations at break were 14% and 16%, respectively.
Example 5
A preparation method of an organic/inorganic hybrid membrane-coated cotton textile comprises the following steps:
(1) firstly, uniformly spraying a sodium phytate solution (the concentration is 35g/L), a zinc chloride solution (the concentration is 18g/L), a potassium polyaspartate solution (the concentration is 17g/L, the molecular weight is M.W to 7000 to 8000) and a nano sepiolite dispersion solution (the concentration is 7g/L, the specific size is that the length of the nano sepiolite is 10 mu m, and the width is 10 nm;);
the specific spraying process comprises the following steps: firstly, respectively filling a sodium phytate solution, a zinc chloride solution, a polyaspartic acid potassium solution and a nano sepiolite dispersion liquid into different spray pots, adjusting the spraying effect of the spray pots to be mist, then spraying the sodium phytate solution, spraying the zinc chloride solution, spraying the polyaspartic acid potassium solution, then placing the mixture into an oven to dry at 90 ℃ for 4.5min, then spraying the nano sepiolite dispersion liquid, and finally continuing to place the mixture into the oven to dry at 90 ℃ for 4.5 min;
the mass ratio of the solute in the sprayed sodium phytate solution, the solute in the potassium polyaspartate solution, the solute in the zinc chloride solution and the dispersoid in the nano sepiolite dispersion liquid is 60:3:15: 8; the thickness of a formed film after spraying the sodium phytate solution, the potassium polyaspartate solution, the zinc chloride solution and the nano sepiolite dispersion liquid is 125 nm;
(2) then drying the sprayed cotton textile at 104 ℃ for 8 min;
(3) and (3) repeating the processes of the steps (1) to (2) for 17 times to obtain the organic/inorganic hybrid film-coated cotton textile.
The finally prepared cotton textile coated with the organic/inorganic hybrid membrane has the surface coated with a plurality of layers of organic/inorganic hybrid membranes, and each layer of organic/inorganic hybrid membrane comprises sodium phytate and transition metal ions (Zn)2+) Potassium polyaspartate and nano sepiolite; in a layer of organic/inorganic hybrid film attached to the surface of the cotton textile, transition metals are arranged between sodium phytate and the cotton textile, between sodium phytate and the nano sepiolite, between polyaspartic acid potassium and the cotton textile and between polyaspartic acid potassium and the nano sepioliteIonic bonds and coordinate bonds of the ions are combined; the organic/inorganic hybrid film coated cotton textile achieves V0 level flame retardance of flame retardance standard UL94, the afterflame time is 3s, the smoldering time is 7s, and the LOI is 26%; the warp and weft breaking strengths were 840N and 360N, respectively, and the warp and weft elongations at break were 14% and 16%, respectively.
Example 6
A preparation method of an organic/inorganic hybrid membrane-coated cotton textile comprises the following steps:
(1) firstly, uniformly spraying a potassium phytate solution (the concentration is 45g/L), a ferric nitrate nonahydrate solution (the concentration is 20g/L), a sodium polyaspartate solution (the concentration is 19g/L, the molecular weight is M.W to 7000 to 8000) and a nano sepiolite dispersion solution (the concentration is 8g/L, the specific size is that the length of the nano sepiolite is 20 mu m, the width is 30 nm);
the specific spraying process comprises the following steps: firstly, respectively filling a potassium phytate solution, a ferric nitrate nonahydrate solution, a sodium polyaspartate solution and a nano sepiolite dispersion liquid into different spray pots, adjusting the spraying effect of the spray pots to be mist, then spraying the potassium phytate solution, spraying the ferric nitrate nonahydrate solution, spraying the sodium polyaspartate solution, then placing the mixture into a drying oven to be dried for 5min at 90 ℃, then spraying a layer of nano sepiolite dispersion liquid, and finally continuously placing the mixture into the drying oven to be dried for 5min at 90 ℃;
the mass ratio of the solute in the sprayed potassium phytate solution, the solute in the sodium polyaspartate solution, the solute in the ferric nitrate nonahydrate solution and the dispersoid in the nano sepiolite dispersion liquid is 60:3:25: 8; spraying potassium phytate solution, sodium polyaspartate solution, ferric nitrate nonahydrate solution and nano sepiolite dispersion liquid to form a film with the thickness of 135 nm;
(2) then drying the sprayed cotton textile at 106 ℃ for 9 min;
(3) and (3) repeating the processes of the steps (1) to (2) for 19 times to obtain the organic/inorganic hybrid film-coated cotton textile.
Finally prepared cotton textile coated with organic/inorganic hybrid membrane and surface of cotton textileCoating multiple layers of organic/inorganic hybrid films, wherein each layer of organic/inorganic hybrid film comprises potassium phytate and transition metal ions (Fe)3+) Sodium polyaspartate and nano sepiolite; in the organic/inorganic hybrid film layer attached to the surface of the cotton textile, potassium phytate and nano sepiolite, sodium polyaspartate and the cotton textile, and sodium polyaspartate and nano sepiolite are combined through ionic bonds and coordination bonds of transition metal ions; the organic/inorganic hybrid film coated cotton textile achieves V0 level flame retardance of flame retardance standard UL94, the afterflame time is 1s, the smoldering time is 7s, and the LOI is 26%; the breaking strength in the warp direction and the breaking strength in the weft direction are 845N and 363N, respectively, and the breaking elongation in the warp direction and the breaking elongation in the weft direction are 14% and 16%, respectively.
Example 7
A preparation method of an organic/inorganic hybrid membrane-coated cotton textile comprises the following steps:
(1) firstly, uniformly spraying a sodium phytate solution (the concentration is 52g/L), a zinc nitrate hexahydrate solution (the concentration is 22g/L), a sodium polyaspartate solution (the concentration is 21g/L, the molecular weight is M.W to 7000 to 8000) and a nano sepiolite dispersion solution (the concentration is 10g/L, the specific size is that the length of the nano sepiolite is 30 mu m, the width is 100 nm;);
the specific spraying process comprises the following steps: firstly, respectively filling a sodium phytate solution, a zinc nitrate hexahydrate solution, a sodium polyaspartate solution and a nano sepiolite dispersion liquid into different spray pots, adjusting the spraying effect of the spray pots to be mist, then spraying the sodium phytate solution, then spraying the zinc nitrate hexahydrate solution, then spraying the sodium polyaspartate solution, then placing the solution in a drying oven to dry for 5min at 90 ℃, then spraying the nano sepiolite dispersion liquid, and finally continuing to place the solution in the drying oven to dry for 5min at 90 ℃;
the mass ratio of solute in the sprayed sodium phytate solution, solute in the sodium polyaspartate solution, solute in the zinc nitrate hexahydrate solution and dispersoid in the nano sepiolite dispersion liquid is 60:6:25: 15; spraying sodium phytate solution, sodium polyaspartate solution, zinc nitrate hexahydrate solution and nano sepiolite dispersion liquid to form a film with the thickness of 150 nm;
(2) then drying the sprayed cotton textile at the drying temperature of 110 ℃ for 10 min;
(3) and (3) repeating the processes of the steps (1) to (2) for 20 times to obtain the organic/inorganic hybrid film-coated cotton textile.
The cotton textile coated with the organic/inorganic hybrid membrane is finally prepared, the surface of the cotton textile is coated with a plurality of layers of organic/inorganic hybrid membranes, and each layer of organic/inorganic hybrid membrane comprises sodium phytate and transition metal ions (Zn) from inside to outside2+) Sodium polyaspartate and nano sepiolite; in the organic/inorganic hybrid film layer attached to the surface of the cotton textile, sodium phytate is combined with nano sepiolite, sodium polyaspartate is combined with the cotton textile, and sodium polyaspartate is combined with nano sepiolite through ionic bonds and coordination bonds of transition metal ions; the organic/inorganic hybrid film coated cotton textile achieves V0 level flame retardance of flame retardance standard UL94, the afterflame time is 0s, the smoldering time is 3s, and the LOI is 26%; the warp and weft breaking strengths were 848N and 365N, respectively, and the warp and weft elongations at break were 14% and 15%, respectively.
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