CN110130104B - Biomass-based flame-retardant real silk fabric and preparation method thereof - Google Patents

Biomass-based flame-retardant real silk fabric and preparation method thereof Download PDF

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CN110130104B
CN110130104B CN201910148962.4A CN201910148962A CN110130104B CN 110130104 B CN110130104 B CN 110130104B CN 201910148962 A CN201910148962 A CN 201910148962A CN 110130104 B CN110130104 B CN 110130104B
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silk fabric
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关晋平
吕仲
陈国强
唐人成
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Suzhou University
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    • DTEXTILES; PAPER
    • D06TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06MTREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M13/00Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment
    • D06M13/244Treating 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 sulfur or phosphorus
    • D06M13/282Treating 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 sulfur or phosphorus with compounds containing phosphorus
    • D06M13/292Mono-, di- or triesters of phosphoric or phosphorous acids; Salts thereof
    • DTEXTILES; PAPER
    • D06TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06MTREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M15/00Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment
    • D06M15/01Treating 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
    • DTEXTILES; PAPER
    • D06TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06MTREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M15/00Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment
    • D06M15/01Treating 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
    • D06M15/03Polysaccharides or derivatives thereof
    • DTEXTILES; PAPER
    • D06TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06MTREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M2101/00Chemical constitution of the fibres, threads, yarns, fabrics or fibrous goods made from such materials, to be treated
    • D06M2101/02Natural fibres, other than mineral fibres
    • D06M2101/10Animal fibres
    • DTEXTILES; PAPER
    • D06TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06MTREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M2200/00Functionality of the treatment composition and/or properties imparted to the textile material
    • D06M2200/30Flame or heat resistance, fire retardancy properties

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Abstract

The invention relates to a biomass-based flame-retardant real silk fabric and a preparation method thereof, wherein the method comprises the following steps: alternately padding a positive charge solution and a negative charge solution on the surface of the real silk fabric in sequence to prepare the biomass-based flame-retardant real silk fabric, wherein the positive charge solution is a chitosan solution with the pH value of 5.0-5.5, and the negative charge solution is a sodium phytate solution with the pH value of 4.0-4.5 and a calcium lignosulfonate solution with the pH value of 4.0-4.5; the padding process comprises the following steps: dipping → taking out → roll extrusion. The prepared biomass-based flame-retardant real silk fabric mainly comprises a real silk fabric, and chitosan, sodium phytate and calcium lignosulfonate deposited on the surface of the real silk fabric, wherein the limit oxygen index is 24-41.5%, the carbon length is 99-110 mm, and the flame-retardant real silk fabric is free of smoldering and afterburning. The preparation method has simple process and high production efficiency, and the prepared product has good flame retardant property and mechanical property and can realize industrial production.

Description

Biomass-based flame-retardant real silk fabric and preparation method thereof
Technical Field
The invention belongs to the technical field of textile finishing, and relates to a biomass-based flame-retardant real silk fabric and a preparation method thereof.
Background
The real silk is praised as 'fibre queen' because of its good moisture absorption, air permeability and comfort, soft luster and excellent health care, and is widely used in various clothes and interior decoration materials. However, most of fire accidents are caused by textiles, and the Limit Oxygen Index (LOI) of real silk is about 23 percent, so that the real silk belongs to combustible fibers. Therefore, the flame-retardant finishing research on the real silk fabric has important practical significance for obtaining good flame-retardant performance.
The electrostatic layer-by-layer self-assembly is a process of forming a molecular aggregate which has a complete structure, relatively stable performance and a certain specific function by spontaneously associating layers in a layer-by-layer alternate deposition mode through weak interaction (such as electrostatic alternate adsorption, hydrogen bonds or covalent bonds) among molecules of each layer. The electrostatic layer-by-layer self-assembly method is mostly realized by adopting an immersion method, which needs a lot of time consumption and is difficult to realize industrial production.
Most of the biomass materials are natural, nontoxic and environment-friendly high molecular compounds. With the continuous enhancement of environmental awareness of people, the application of biomass materials with flame retardant effect to the flame retardant finishing of textiles by utilizing the technology of simple electrostatic layer-by-layer self-assembly process equipment and mild preparation conditions has become one of the hot topics of current research.
Patent ZL201310284364.2 discloses a technology of preparing flame-retardant real silk fabric by a static layer-by-layer self-assembly method, which mainly adopts 1-2% sodium phytate and 0.5-1% low molecular weight chitosan solution as finishing liquid, alternately soaks the fabric in the two solutions, washes and dries, repeats 5-20 positive and negative ions alternate deposition, namely completes modification, after 20 alternate depositions of 1% chitosan and 1% sodium phytate, the limit oxygen index of the real silk fabric can reach 32%, but the warp-wise strength and weft-wise strength of the real silk fabric are both reduced, wherein the weft-wise reduction is more. Patent ZL201410162821.5 discloses a method for preparing flame-retardant materials such as fabric, plastic and wood by self-assembling polyelectrolyte nano flame-retardant coating layer by layer, which is mainly to prepare the flame-retardant material by acidifying the matrix and then alternately depositing anionic and cationic polyelectrolyte solutions. Although the methods can endow the material with certain flame retardant property, the flame retardant property is still to be further improved, and the treatment processes (soaking, washing and drying) are too long in time and too low in efficiency.
Therefore, the flame retardant treatment method for real silk fabrics, which has the advantages of simple treatment process, high efficiency, environmental friendliness and excellent flame retardant property of products, is urgently needed to be provided.
Disclosure of Invention
The invention aims to solve the problems of poor environment friendliness, complex treatment process, low efficiency and incapability of achieving a high-level flame retardant property of a product in the prior art, and provides a real silk fabric flame retardant treatment method which is simple in treatment process, high in efficiency, environment-friendly and excellent in flame retardant property of the product.
In order to achieve the purpose, the invention adopts the technical scheme that:
a biomass-based flame-retardant real silk fabric mainly comprises a real silk fabric, and chitosan, sodium phytate and calcium lignosulfonate deposited on the surface of the real silk fabric. The chitosan with higher molecular weight on the fabric is combined with sodium phytate and calcium lignosulphonate through electrostatic acting force, so that the connection is firm, the durability is strong, the flame retardant property of the real silk fabric is greatly improved, and the mechanical property of the real silk fabric is also improved to a certain extent.
As a preferred technical scheme:
according to the biomass-based flame-retardant real silk fabric, the limit oxygen index of the biomass-based flame-retardant real silk fabric is 24% -41.5%, the carbon length is 99-110 mm, and the biomass-based flame-retardant real silk fabric is free of smoldering and afterburning phenomena and strong damage. By adopting a reported bio-based flame-retardant modification method, 1 wt% of chitosan solution and 1 wt% of sodium phytate solution are sequentially soaked in real silk electric power textile, the real silk electric power textile is assembled on the surface of the textile layer by layer, after 10 times of alternate deposition, the limit oxygen index of the manufactured textile is 28.3% and is lower than that of the invention, and the warp direction strength and the weft direction strength are both reduced (the warp direction strength is reduced from 338.1N to 333.6N, and the weft direction strength is reduced from 296.8N to 259.7N).
According to the biomass-based flame-retardant real silk fabric, the deposition is that the positive charge layer and the negative charge layer are alternately deposited, the positive charge layer is a chitosan layer, and the negative charge layer is a sodium phytate layer and a calcium lignosulfonate layer. The chitosan layer of the invention has positive charges, the sodium phytate layer and the calcium lignosulfonate layer have negative charges, and the chitosan layer is respectively connected with the sodium phytate layer and the calcium lignosulfonate layer in an electrostatic manner and alternately deposited. The chitosan layer and the real silk fabric layer are connected through electrostatic acting force and intermolecular acting force.
According to the biomass-based flame-retardant real silk fabric, all layers on the surface of the real silk fabric are assembled together to form a composite film layer. Compared with a layer-by-layer assembly structure formed by dipping, the layer-by-layer assembly structure formed by alternate dipping and rolling is more uniform, all layers can be assembled together to form a composite film layer, the conventional electrostatic layer-by-layer self-assembly method adopts the procedures of dipping (rolling) positive ions, cleaning, dipping (rolling) negative ions and cleaning, is complex to operate and is suitable for surface modification of metal or silicon wafers.
The biomass-based flame-retardant real silk fabric is characterized in that the composite film layer is composed of n unit layers, wherein n is 1-15, and each unit layer is composed of a chitosan layer, calcium lignosulfonate, a chitosan layer and a sodium phytate layer which are sequentially arranged. And n is larger than 15, the hand feeling of the real silk fabric is hard. N is preferably 3-5, because the larger the value of n is, although the flame retardant and mechanical properties are better, the larger the value of n is, and the larger the value of n is, the larger the value of n is.
According to the biomass-based flame-retardant real silk fabric, the molecular weight of the chitosan is more than 41 ten thousand daltons, the molecular weight of the chitosan is too low, and the assembly fastness is not sufficient; molecular weights are too large, e.g., above a million, and chitosan has too high a viscosity and poor solubility.
The invention also provides a method for preparing the biomass-based flame-retardant real silk fabric, which comprises the steps of alternately padding a positive charge solution and a negative charge solution on the surface of the real silk fabric in sequence to prepare the biomass-based flame-retardant real silk fabric;
the positive charge solution is a chitosan solution with the pH value of 5.0-5.5, the negative charge solution is a sodium phytate solution with the pH value of 4.0-4.5 and a calcium lignosulfonate solution with the pH value of 4.0-4.5, and the negative charge solution can also be a mixed solution of the sodium phytate solution and the calcium lignosulfonate solution;
the padding process comprises the following steps: dipping → taking out → rolling extrusion, and the process of alternate dipping and rolling comprises the following steps: dipping the positive charge solution → taking out → rolling extrusion → dipping the negative charge solution → taking out → rolling extrusion, repeating the required number of assembly layers, and then drying.
The invention simplifies the prior padding process by omitting the water washing step, saves the time cost, improves the production efficiency and prepares the real silk fabric with good flame retardant effect and good mechanical property. And because the raw materials used in the invention are all environment-friendly products, the environment is not adversely affected.
As a preferred technical scheme:
according to the method, the real silk fabric is white-refined real silk fabric, the fabric can be firmly combined with chitosan through white refining, the concentration of the chitosan solution is 0.5-1.0 wt%, the concentration of the sodium phytate solution is 0.5-1.0 wt%, and the concentration of the calcium lignosulphonate solution is 0.5-1.0 wt%. The concentrations of the chitosan solution, the sodium phytate solution and the calcium lignosulfonate solution are too low to meet the requirement of the flame retardant property of the product; the concentrations of the chitosan solution and the riboflavin sodium phosphate solution are too high, which causes the waste of cost.
According to the method, the dipping time is less than 1min, the mangle squeezing rate of the rollers is 90-100%, and the mangle squeezing rates of the rollers at all stages in the alternate padding process are the same or different. The mangle ratio of roller extrusion is too low, the fire retardant is less rolled into the fabric, and the fire retardant performance of the fabric is influenced.
According to the method, the pH values of the chitosan solution, the sodium phytate solution and the calcium lignosulfonate solution are adjusted by using acetic acid and sodium hydroxide, only the acetic acid and the sodium hydroxide are taken as examples, other solvents can be used for adjusting the pH value as long as other substances which may influence the performance of products are not introduced, and after the alternate padding is finished, the real silk fabric is dried for 5min at the temperature of 90 ℃. The drying temperature is too high, the real silk is easy to turn yellow, and the attractiveness of the product is influenced; the drying temperature is too low, the drying efficiency is too low, and the required drying time is too long.
The invention mechanism is as follows:
according to the invention, chitosan solution, sodium phytate solution and calcium lignosulfonate solution with specific pH value and molecular weight are alternately padded on the surface of the real silk fabric to realize layer-by-layer assembly, wherein the negatively charged real silk fabric layer is combined with the positively charged chitosan layer through electrostatic acting force and intermolecular acting force, the positively charged chitosan layer is combined with the negatively charged sodium phytate layer or calcium lignosulfonate layer through electrostatic acting force, and the chitosan layer and the sodium phytate layer or the calcium lignosulfonate layer are sequentially deposited to realize uniform deposition of positive and negative charge substances on the surface of the real silk fabric. The pH values of the chitosan solution, the sodium phytate solution and the calcium lignosulfonate solution are 5.0-5.5, 4.0-4.5 and 4.0-4.5 respectively, so that the chitosan solution, the sodium phytate solution and the calcium lignosulfonate solution have proper solubility and charge density. The invention simplifies the prior padding process, saves the time cost and prepares the flame-retardant real silk fabric with equivalent and even better flame-retardant effect.
Has the advantages that:
(1) the biomass-based flame-retardant real silk fabric disclosed by the invention is good in flame retardant property, the assembling agent can be uniformly deposited on the surface of the fabric, the utilization rate of the assembling agent is obviously improved, the mechanical property of the real silk fabric is greatly improved, and the biomass-based flame-retardant real silk fabric has a great application prospect;
(2) the preparation method of the biomass-based flame-retardant real silk fabric is simple in process, high in production efficiency and capable of realizing industrial production, and the raw materials are all bio-based materials and are environment-friendly.
Drawings
FIG. 1 is an SEM image of the surface of an untreated white silk fabric;
FIG. 2 is a SEM image of the surface of a fabric prepared according to example 1 of the present invention;
FIG. 3 is a SEM image of the surface of a fabric prepared according to example 2 of the present invention;
FIG. 4 is a SEM image of the surface of a fabric prepared according to example 3 of the present invention;
FIG. 5 is a SEM photograph of the surface of a fabric prepared according to example 4 of the present invention;
wherein, 1QL represents the fabric prepared in example 1 (the flame-retardant real silk fabric prepared by 1-time alternate padding), 5QL represents the fabric prepared in example 2 (the flame-retardant real silk fabric prepared by 5-time alternate padding), 10QL represents the fabric prepared in example 3 (the flame-retardant real silk fabric prepared by 10-time alternate padding), and 15QL represents the fabric prepared in example 4 (the flame-retardant real silk fabric prepared by 15-time alternate padding).
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 a biomass-based flame-retardant real silk fabric comprises the following specific steps:
(1) soaking the white-refined real silk fabric in a chitosan solution with the concentration of 0.5 wt% and the pH value of 5.0 for 0.8min, taking out the white-refined real silk fabric, and then performing roll extrusion under the condition of the mangling press rate of 100%, wherein the pH value of the chitosan solution is adjusted by acetic acid, the weight-average molecular weight of chitosan is 41 kilodaltons, and the white-refined real silk fabric is subjected to white refining treatment and has the gram weight of 36g/m2The electric textile of (1);
(2) dipping the white silk fabric treated in the step (1) in a sodium phytate solution with the concentration of 0.5 wt% and the pH value of 4.0 for 0.7min, taking out the white silk fabric, and extruding the white silk fabric by using a roller under the condition that the mangle rolling rate is 100%, wherein the pH value of the sodium phytate solution is adjusted by using acetic acid;
(3) soaking the white-silk-like fabric treated in the step (2) in the chitosan solution consistent with the step (1) again, taking out the fabric, and extruding the fabric by a roller under the condition that the mangle rolling rate is 100%;
(4) dipping the white silk fabric treated in the step (3) in calcium lignosulfonate solution with the concentration of 1.0wt% and the pH value of 4.0 for 0.9min, taking out, and then rolling and extruding under the condition that the mangle rolling rate is 90%, wherein the pH value of the calcium lignosulfonate solution is adjusted by sodium hydroxide;
the white-silk-like fabric processed in the steps (1) to (4) is subjected to one-time alternate padding, and is marked as a QL (quantum dot), namely n is 1 QL;
(5) and drying the white-refined real silk fabric for 5min at the temperature of 90 ℃ to obtain the biomass-based flame-retardant real silk fabric.
The limit oxygen index of the prepared biomass-based flame-retardant real silk fabric is 24%, the real silk fabric is burnt and polished within 12s in a vertical burning test, smoldering and afterburning phenomena are avoided, and the mechanical properties are shown in table 1.
Example 2
A preparation method of a biomass-based flame-retardant real silk fabric comprises the following specific steps:
(1) soaking the white-refined real silk fabric in a chitosan solution with the concentration of 0.5 wt% and the pH value of 5.0 for 0.6min, taking out, and then carrying out roller extrusion under the condition of the mangling press rate of 100%, wherein the pH value of the chitosan solution is adjusted by acetic acid, the weight-average molecular weight of chitosan is 42 kilodaltons, and the white-refined real silk fabric is subjected to white refining treatment and has the gram weight of 36g/m2The electric textile of (1);
(2) dipping the white silk fabric treated in the step (1) in a sodium phytate solution with the concentration of 0.5 wt% and the pH value of 4.0 for 0.7min, taking out the white silk fabric, and extruding the white silk fabric by using a roller under the condition that the mangle rolling rate is 95%, wherein the pH value of the sodium phytate solution is adjusted by using acetic acid;
(3) soaking the white-silk-like fabric treated in the step (2) in the chitosan solution consistent with the step (1) again, taking out the fabric, and extruding the fabric by a roller under the condition that the mangle rolling rate is 100%;
(4) dipping the white silk fabric treated in the step (3) in calcium lignosulfonate solution with the concentration of 1.0wt% and the pH value of 4.0 for 0.5min, taking out, and then rolling and extruding under the condition that the mangle rolling rate is 95%, wherein the pH value of the calcium lignosulfonate solution is adjusted by sodium hydroxide;
(5) finishing one-time alternate padding, namely marking as a QL, and repeating alternate padding until n is 5 QL;
(6) and drying the white-refined real silk fabric for 5min at the temperature of 90 ℃ to obtain the biomass-based flame-retardant real silk fabric.
The limit oxygen index of the prepared biomass-based flame-retardant real silk fabric is 30.1%, the carbon length is 110mm, smoldering and afterflame phenomena are avoided, and the mechanical properties are shown in Table 1.
Example 3
A preparation method of a biomass-based flame-retardant real silk fabric comprises the following specific steps:
(1) soaking the white-refined real silk fabric in a chitosan solution with the concentration of 1.0wt% and the pH value of 5.0 for 0.6min, taking out, and then carrying out roller extrusion under the condition of the mangling press rate of 92%, wherein the pH value of the chitosan solution is adjusted by acetic acid, the weight-average molecular weight of chitosan is 41 kilodaltons, and the white-refined real silk fabric is subjected to white refining treatment and has the gram weight of 36g/m2The electric textile of (1);
(2) dipping the white silk fabric treated in the step (1) in sodium phytate solution with the concentration of 1.0wt% and the pH value of 4.0 for 0.5min, taking out, and extruding by using a roller under the condition that the mangle rolling rate is 92%, wherein the pH value of the sodium phytate solution is adjusted by using acetic acid;
(3) soaking the white-silk-like fabric treated in the step (2) in the chitosan solution consistent with the step (1) again, taking out the fabric, and extruding the fabric by a roller under the condition that the mangle rolling rate is 92%;
(4) dipping the white silk fabric treated in the step (3) in calcium lignosulfonate solution with the concentration of 1.0wt% and the pH value of 4.0 for 0.8min, taking out, and then rolling and extruding under the condition that the mangle rolling rate is 92%, wherein the pH value of the calcium lignosulfonate solution is adjusted by sodium hydroxide;
(5) finishing one-time alternate padding, namely marking as a QL, and repeating alternate padding until n is 10 QL;
(6) and drying the white-refined real silk fabric for 5min at the temperature of 90 ℃ to obtain the biomass-based flame-retardant real silk fabric.
The limit oxygen index of the prepared biomass-based flame-retardant real silk fabric is 33.8%, the carbon length is 100mm, smoldering and afterflame phenomena are avoided, and the mechanical properties are shown in table 1.
Example 4
A preparation method of a biomass-based flame-retardant real silk fabric comprises the following specific steps:
(1) soaking the white-refined real silk fabric in a chitosan solution with the concentration of 1.0wt% and the pH value of 5.0 for 0.6min, taking out, and then carrying out roller extrusion under the condition of the mangling press rate of 98%, wherein the pH value of the chitosan solution is adjusted by acetic acid, the weight-average molecular weight of chitosan is 43 kilodaltons, and the white-refined real silk fabric is subjected to white refining treatment and has the gram weight of 36g/m2The electric textile of (1);
(2) dipping the white silk fabric treated in the step (1) in sodium phytate solution with the concentration of 1.0wt% and the pH value of 4.0 for 0.5min, taking out, and extruding by using a roller under the condition that the mangle rolling rate is 100%, wherein the pH value of the sodium phytate solution is adjusted by using acetic acid;
(3) soaking the white-silk-like fabric treated in the step (2) in the chitosan solution consistent with the step (1) again, taking out the fabric, and extruding the fabric by a roller under the condition that the mangle rolling rate is 94%;
(4) dipping the white silk fabric treated in the step (3) in calcium lignosulfonate solution with the concentration of 1.0wt% and the pH value of 4.0 for 0.8min, taking out, and then rolling and extruding under the condition that the mangle rolling rate is 100%, wherein the pH value of the calcium lignosulfonate solution is adjusted by sodium hydroxide;
(5) finishing one-time alternate padding, namely marking as a QL, and repeating alternate padding until n is 15 QL;
(6) and drying the white-refined real silk fabric for 5min at the temperature of 90 ℃ to obtain the biomass-based flame-retardant real silk fabric.
The limit oxygen index of the prepared biomass-based flame-retardant real silk fabric is 41.5%, the carbon length is 99mm, smoldering and afterflame phenomena are avoided, and the mechanical properties are shown in table 1.
Fig. 1 to 5 are SEM images of the number of dipping units versus the number of silk fabrics (silk) before and after flame-retardant finishing, and it can be seen from the SEM images that the untreated white silk fabric (i.e., fig. 1) has well-defined fiber tows and a clean and smooth surface. Along with the increase of the number of the dipping units, the surface of the real silk is covered by the assembling agent, and the thickness is increased along with the increase of the number of the dipping units, which shows that the assembling agent is successfully and uniformly deposited on the surface of the real silk fabric after being assembled and finished.
Table 1 shows that the breaking strength of the real silk fabric after the assembly and the finishing is slightly improved, and the breaking strength and the breaking elongation of the fabric are correspondingly and slowly increased with the increase of the number of the dipping units, which indicates that a thicker and uniform film is formed on the surface of the real silk fabric after the real silk fabric is finished by the layer-by-layer self-assembly of chitosan, sodium phytate and calcium lignosulfonate, and the breaking strength of the film can be improved by the film layer. It can also be seen from the table that the bending stiffness of the real silk fabric increases with the number of the dipping units, mainly because the quantity of the assembling agent on the real silk fabric increases, but the hand feeling of the real silk fabric is affected by the quantity of the assembling agent on the real silk fabric. The warp breaking strength of the assembled 5QL silk fabric is improved by 5.53%, the breaking elongation is improved by 5.68%, and although the flexibility is reduced due to the increase of the bending rigidity, the use requirement can be basically met. Therefore, in view of the above, the 5QL can be assembled to satisfy the requirement of the taking performance.
TABLE 1 physical Properties of real Silk fabrics before and after flame-retardant finishing
Figure BDA0001980962100000071
Table 2 shows the comparison of the element contents before and after changing the number of the dipping units, and it can be seen that the surface of the untreated real silk fabric only contains C, O and N elements. The content of N, P and S element on the surface of the assembled real silk fabric is increased, and the content is increased along with the increase of the number of the assembling layers, which indicates that the assembling agent is successfully assembled on the real silk fabric. Due to the P-N synergistic intumescent flame retardant mechanism, the real silk fabric has good flame retardant effect.
Table 2 shows the contents of elements before and after flame-retardant finishing
Figure BDA0001980962100000072
Tests prove that the assembling agent is uniformly deposited on the surface of the real silk fabric by alternately padding the positive charge solution and the negative charge solution on the surface of the real silk fabric, so that the flame retardant effect is greatly improved, the thermal stability of the finished real silk fabric is better, and the assembling agent forms a film on the surface of the real silk fabric, so that the mechanical property of the fabric is improved. The invention omits the water washing step in the padding treatment process, namely, the padding-padding process is adopted, and the padding-padding process is not washed after each layer of positive or negative ions is assembled, so that an assembled film can be formed on the surface of the fabric and in gaps among fabric tissues, and the flame retardant property of the fabric can be further improved.
Example 5
A preparation method of a flame-retardant real silk fabric based on biomass, which is basically the same as in example 4, and is characterized in that the pH values of a chitosan solution, a sodium phytate solution and a calcium lignosulfonate solution are 5.5, 4.5 and 4.5 respectively. The prepared biomass-based flame-retardant real silk fabric has the limiting oxygen index of 40.2 percent, the carbon length of 100mm, no smoldering and afterflame phenomena and no strong damage.

Claims (6)

1. A flame-retardant real silk fabric based on biomass is characterized in that: the silk fabric mainly comprises a silk fabric, and chitosan, sodium phytate and calcium lignosulphonate which are deposited on the surface of the silk fabric; the deposition is that a positive charge layer and a negative charge layer are alternately deposited, the positive charge layer is a chitosan layer, and the negative charge layer is a sodium phytate layer and a calcium lignosulfonate layer; all layers on the surface of the real silk fabric are assembled together to form a composite membrane layer; the composite film layer is composed of n unit layers, wherein n = 1-15, and each unit layer is composed of a chitosan layer, calcium lignosulphonate, a chitosan layer and a sodium phytate layer which are sequentially arranged; the biomass-based flame-retardant real silk fabric has the limiting oxygen index of 24-41.5%, the carbon length of 99-110 mm, no smoldering and afterflame phenomena and no strong damage relative to the real silk fabric.
2. The biomass-based flame-retardant real silk fabric according to claim 1, wherein the molecular weight of the chitosan is more than 41 ten thousand daltons.
3. A process for preparing a biomass-based flame-retardant real silk fabric according to claim 1 or 2, characterized in that: alternately padding a positive charge solution and a negative charge solution on the surface of the real silk fabric in sequence to prepare the biomass-based flame-retardant real silk fabric;
the positive charge solution is a chitosan solution with the pH value of 5.0-5.5, and the negative charge solution is a sodium phytate solution with the pH value of 4.0-4.5 and a calcium lignosulphonate solution with the pH value of 4.0-4.5;
the padding process comprises the following steps: dipping → taking out → roll extrusion.
4. The method according to claim 3, wherein the real silk fabric is a white-off real silk fabric, the concentration of the chitosan solution is 0.5-1.0 wt%, the concentration of the sodium phytate solution is 0.5-1.0 wt%, and the concentration of the calcium lignosulfonate solution is 0.5-1.0 wt%.
5. The method according to claim 3, wherein the dipping time is less than 1min, the mangle ratio of the roller extrusion is 90-100%, and the mangle ratio of the roller extrusion at each stage in the alternate padding process is the same or different.
6. The method as claimed in claim 3, wherein the pH values of the chitosan solution, the sodium phytate solution and the calcium lignosulfonate solution are adjusted by using acetic acid and sodium hydroxide, and after the alternate padding is finished, the real silk fabric is dried for 5min at the temperature of 90 ℃.
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CN110616565B (en) * 2019-10-30 2021-04-09 河南大学 Preparation method of nylon 66 textile surface nano fireproof coating
CN112458745B (en) * 2020-09-29 2022-01-07 东华大学 Method for preparing flexible inorganic semiconductor textile composite material by padding
CN115198527B (en) * 2022-07-04 2023-09-26 同济大学 Layer-by-layer self-assembled flame-retardant fabric based on full biomass flame-retardant system and preparation method thereof

Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101613943A (en) * 2009-07-17 2009-12-30 东华大学 A kind of preparation method of layer-by-layer self-assembly polyaniline amine/nylon composite conductive fabric
CN103321044A (en) * 2013-07-08 2013-09-25 苏州大学 Flame-retardant pure silk and preparation method thereof
CN107938340A (en) * 2017-11-27 2018-04-20 无锡昊瑜节能环保设备有限公司 A kind of flame-proof finishing process of real silk fabric
CN108893975A (en) * 2018-07-30 2018-11-27 嘉兴学院 A kind of method that graphene is used for the arrangement of polyamide fibre product
CN109281168A (en) * 2018-10-31 2019-01-29 南通纺织丝绸产业技术研究院 Soluble poly pentalyte and its method to protein fibre flame-proof treatment

Family Cites Families (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4857638A (en) * 1987-12-28 1989-08-15 Domtar Inc. Lignin having nitrogen and sulfur and process therefor employing thiourea

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101613943A (en) * 2009-07-17 2009-12-30 东华大学 A kind of preparation method of layer-by-layer self-assembly polyaniline amine/nylon composite conductive fabric
CN103321044A (en) * 2013-07-08 2013-09-25 苏州大学 Flame-retardant pure silk and preparation method thereof
CN107938340A (en) * 2017-11-27 2018-04-20 无锡昊瑜节能环保设备有限公司 A kind of flame-proof finishing process of real silk fabric
CN108893975A (en) * 2018-07-30 2018-11-27 嘉兴学院 A kind of method that graphene is used for the arrangement of polyamide fibre product
CN109281168A (en) * 2018-10-31 2019-01-29 南通纺织丝绸产业技术研究院 Soluble poly pentalyte and its method to protein fibre flame-proof treatment

Non-Patent Citations (4)

* Cited by examiner, † Cited by third party
Title
"Effect of Fully Biobased Coatings Constructed via Layer-by-LayerAssembly of Chitosan and Lignosulfonate on the Thermal, Flame Retardant, and Mechanical Properties of Flexible Polyurethane Foam";Ying Pan等;《American Chemical Society》;20151224;第1431-1438页 *
"采用静电层层自组装法制备阻燃蚕丝织物的工艺条件及产品性能测试";徐婕等;《蚕业科学》;20140623;第75-80页 *
Phytic acid–lignin combination: A simple and efficient route for;L. Costes et al.;《European Polymer Journal》;20170714;第270-285页 *
静电自组装法制备阻燃抗菌染色蚕丝织物;沈家力等;《印染》;20150603;第1-5页 *

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