CN109371660B - Flame-retardant silk and preparation method and application thereof - Google Patents
Flame-retardant silk and preparation method and application thereof Download PDFInfo
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- CN109371660B CN109371660B CN201811270759.6A CN201811270759A CN109371660B CN 109371660 B CN109371660 B CN 109371660B CN 201811270759 A CN201811270759 A CN 201811270759A CN 109371660 B CN109371660 B CN 109371660B
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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
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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
- D06M13/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment
- D06M13/10—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment with compounds containing oxygen
- D06M13/224—Esters of carboxylic acids; Esters of carbonic acid
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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
- D06M2101/00—Chemical constitution of the fibres, threads, yarns, fabrics or fibrous goods made from such materials, to be treated
- D06M2101/02—Natural fibres, other than mineral fibres
- D06M2101/10—Animal fibres
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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
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- Textile Engineering (AREA)
- Treatments For Attaching Organic Compounds To Fibrous Goods (AREA)
- Chemical Or Physical Treatment Of Fibers (AREA)
Abstract
The invention discloses a method for preparing flame-retardant silk, which comprises the following steps: immersing silk into a tannic acid solution with the pH value of 3-4, heating to 80-90 ℃, and carrying out heat preservation treatment; and immersing the treated silk into a metal salt solution of 2-6g/L, and heating to 50-70 ℃ for treatment to obtain the flame-retardant silk. The method of the invention endows the silk with good flame retardant performance under the condition of not adding traditional flame retardant containing nitrogen, phosphorus and halogen elements, and can avoid the problem of environmental pollution caused by the traditional flame retardant in the production and use processes of the flame-retardant silk and the nitrogen, phosphorus and halogen elements after the flame-retardant silk is discarded. The method has the advantages of environmental protection, high efficiency, simplicity and feasibility.
Description
Technical Field
The invention relates to the technical field of textile finishing, in particular to a method for preparing flame-retardant silk and the flame-retardant silk prepared by the method.
Background
Silk is one of the most common natural protein fibers, and is popular with consumers due to its soft and natural luster, unique silky feeling, good health care and comfort. The silk textile is often used for manufacturing high-grade clothes and ornaments, and the silk ornaments and parts of daily-use clothes have higher requirements on flame retardant property. The silk as natural protein fiber can not be subjected to flame retardant modification by a method of blending and spinning with a flame retardant, and can only achieve the purpose of flame retardance by the post-finishing processing of printing and dyeing. Good flame retardant finish, in addition to providing flame retardant functionality, must be non-toxic, smoke less, resistant to washing and dry cleaning to a certain extent, and not interfere with the original good quality of silk.
The silk is treated by a stannic acid or boric acid-borax dipping method in the early stage, so that the silk is not resistant to washing although the flame retardant effect is good. Halogen flame retardants have been used for flame retardant finishing of silk, but have been banned for later use due to toxicity problems. Phosphorus-nitrogen flame retardants for cotton have also been used in flame retardant finishing of silk, and can impart good flame retardant properties and water-washing resistance to silk, but have disadvantages of high processing cost, complex process, hard and yellow hand feeling of the obtained silk, and free formaldehyde release. At present, the Zirpro process widely applied to wool flame-retardant finishing is also applied to silk to a certain extent, the flame-retardant performance of the silk can be effectively improved by performing flame-retardant finishing on the silk through metal complexes such as titanium and zirconium, but the variety of the applied metal ions is few, the price is relatively high, and the washability of the flame-retardant function is not good enough. As phosphorus element can cause eutrophication in water, the halogen element flame retardant can release toxic gas in the using process, thereby harming the environment and human body. Therefore, paying attention to the environmental problem, developing a flame retardant technology which is green, friendly, economical, applicable and simple in application process is a problem to be solved urgently in the field.
Disclosure of Invention
The invention aims to solve the technical problem of providing a method for preparing flame-retardant silk, which is simple in preparation method and good in flame-retardant effect.
In order to solve the technical problem, the invention provides the following scheme: a method for preparing flame-retardant silk comprises the following steps:
s1, immersing silk into a tannic acid solution with the pH value of 3-4, heating to 80-90 ℃ and carrying out heat preservation treatment;
and S2, immersing the silk processed in the step S1 into a metal salt solution of 2-6g/L, and heating to 50-70 ℃ for processing to obtain the flame-retardant silk.
The tannic acid is derived from plant tissues, contains carboxyl, can be adsorbed on silk under the weak acidic condition, and is combined with the silk through ionic bonds; after tannic acid is adsorbed on silk, metal salt treatment is carried out, and metal ions can be complexed with tannic acid adsorbed on the silk and silk fiber, so that the thermal degradation process during silk combustion is changed, and the flame retardant effect is achieved. The silk treated by the combination of the tannic acid and the metal salt has good flame retardant property and excellent washability.
Further, the method comprises the following steps: the time of the heat preservation treatment in the step S1 is 45-75 min.
Further, the method comprises the following steps: the treatment time at 50-70 ℃ in the step S2 is 20-40 min.
Further, the method comprises the following steps: in the step S1, the amount of tannic acid is 10-30% of the relative weight of silk.
Further, the method comprises the following steps: the metal salt is one or more of ferrous sulfate, ferric sulfate, titanium sulfate or calcium sulfate.
The invention further provides the flame-retardant silk prepared by the method.
The invention further provides application of the flame-retardant silk prepared by the method in the aspect of spinning.
The invention has the beneficial effects that:
1. the tannic acid used in the invention is derived from plant tissues and is an environment-friendly natural compound.
2. The flame-retardant finishing method used in the invention is a brand-new flame-retardant method and technology, the flame-retardant finishing process is simple to operate and has obvious effect, and the used metal ions are easy to obtain and have low price.
3. Under the condition that traditional nitrogen, phosphorus and halogen element flame retardants are not added, the silk can be endowed with good flame retardant performance, the durability of the flame retardant function is excellent, and the problem of environmental pollution caused by the use of the traditional flame retardants in the production and use processes of the flame retardant silk and nitrogen, phosphorus and halogen elements after the flame retardant silk is discarded can be solved. The method has the advantages of environmental protection, high efficiency, simplicity and feasibility.
Detailed Description
The present invention is further described below in conjunction with specific examples to enable those skilled in the art to better understand the present invention and to practice it, but the examples are not intended to limit the present invention.
In the following examples of the invention, the flame retardant property of the silk fabric is measured according to GB/T5454-1997 oxygen index method for textile combustion performance test and GB/T5455-2014-measurement of the smoldering length and the afterflame time of the textile combustion performance in the vertical direction. The washing method of the flame-retardant silk fabric is carried out according to the standard GB/T3921-. And repeating the water washing to the required water washing times.
Example 1
S1, dissolving 20% (relative weight to silk) of tannic acid in water, stirring at normal temperature for 10min, and adjusting pH to 4 with citric acid/disodium hydrogen phosphate buffer solution; soaking silk in the above tannic acid solution, heating to 90 deg.C, keeping the temperature for 45min, taking out silk, cleaning, and oven drying.
And S2, immersing the silk treated by the tannic acid into a ferrous sulfate or ferric sulfate solution of 2g/L, treating at 70 ℃ for 20min, and washing and drying to obtain the durable silk with the flame retardant function.
The limit oxygen index of the silk treated by the tannic acid and the ferrous sulfate is 27.5 percent, and the damage length is only 11.0 cm; the limit oxygen index of the silk treated by the combination of the tannic acid and the ferric sulfate is 27.6 percent, and the damage length is only 11.1 cm. The silk treated by the tannic acid and the ferrous sulfate or the ferric sulfate meets the requirement of B1-grade flame retardant performance (the damage length is less than 15cm) in GB/T17591-2006 flame retardant textiles in China.
Example 2
S1, dissolving 20% (relative weight to silk) of tannic acid in water, stirring at normal temperature for 10min, and adjusting pH to 3 with citric acid/disodium hydrogen phosphate buffer solution; soaking silk in the above tannic acid solution, heating to 80 deg.C, keeping the temperature for 75min, taking out silk, cleaning, and oven drying.
And S2, immersing the silk treated by the tannic acid into 6g/L calcium sulfate or titanium sulfate solution, treating at 50 ℃ for 40min, cleaning and drying to obtain the durable silk with the flame retardant function.
The limit oxygen index of the silk treated by the tannic acid and the calcium sulfate is 27.5 percent, and the damage length is only 12.3 cm; the limit oxygen index of the silk treated by the combination of the tannic acid and the titanium sulfate is 28.5 percent, and the damage length is only 10.0 cm. The silk treated by the tannic acid and the calcium sulfate or the titanium sulfate meets the requirement of B1-grade flame retardant performance in GB/T17591-2006 flame retardant textile in China.
Example 3
S1, respectively dissolving 10%, 20% and 30% (relative weight to silk) of tannic acid in water, stirring at room temperature for 10min, and adjusting pH of the solution to 3 with citric acid/disodium hydrogen phosphate buffer solution; respectively soaking silk in the above tannic acid solution, heating to 90 deg.C, keeping the temperature for 60min, taking out silk, cleaning, and oven drying.
S2, immersing the silk treated by the tannic acid into a ferrous sulfate solution of 2g/L, treating at 60 ℃ for 30min, cleaning and drying to obtain the durable silk with the flame retardant function.
As comparative examples, silk was treated with ferrous sulfate alone: soaking silk fabric in 2g/L ferrous sulfate solution, and treating at 70 deg.C for 30 min; treatment of silk with tannic acid alone: the silk fabric was immersed in 20% (relative weight to silk) tannic acid solution and treated at 90 ℃ for 60 min.
The untreated and treated silk fabrics were tested for flame retardant properties and the results are shown in table 1.
TABLE 1 flame retardancy of Silk fabrics
Table 1 shows that: the limiting oxygen index of the silk treated by ferrous sulfate alone is 25.1%, the silk is completely combusted in a vertical combustion test, and the damage length is 30.0 cm; the limiting oxygen index of silk treated with tannic acid alone was 26.1%, and the length of damage upon vertical combustion was 19.5 cm; the silk treated by ferrous sulfate or tannic acid alone can not meet the requirement of B1 level flame retardant performance in GB/T17591 and 2006 flame retardant fabrics in China. The limit oxygen index of the silk treated by the combination of 10%, 20% and 30% tannic acid solution and 2g/L ferrous sulfate is 26.9% to 27.9%, the damage length is about 11cm during vertical combustion, and the requirements of B1-level flame retardant performance in GB/T17591 and 2006 flame retardant fabric in China are met.
Example 4
The flame-retardant treatment of the silk fabric was carried out as described in example 1, and the resulting flame-retardant functional silk was subjected to a wash resistance test, the results of which are shown in Table 2.
TABLE 2 washable property of flame-retardant Silk Fabric
Table 2 shows that after repeated washing, the limit oxygen index of the flame-retardant silk is changed very little, and the damage length of the flame-retardant silk is still less than 15cm during vertical burning, which indicates that the flame-retardant effect of the silk prepared by the method has excellent washability or washing durability.
The above examples show that the method for preparing flame-retardant silk according to the present invention can impart good flame-retardant property to silk, and the water washing durability of the flame-retardant function is excellent. The method has the advantages of environmental protection, high efficiency, simplicity and feasibility.
The method of the invention endows the silk with good flame retardant performance under the condition of not adding traditional flame retardant containing nitrogen, phosphorus and halogen elements, and can avoid the problem of environmental pollution caused by the traditional flame retardant in the production and use processes of the flame-retardant silk and the nitrogen, phosphorus and halogen elements after the flame-retardant silk is discarded. The method has the advantages of environmental protection, high efficiency, simplicity and feasibility.
The tannic acid is derived from plant tissues, contains carboxyl, can be adsorbed on silk under the weak acidic condition, and is combined with the silk through ionic bonds; after tannic acid is adsorbed on silk, metal salt treatment is carried out, and metal ions can be complexed with tannic acid adsorbed on the silk and silk fiber, so that the thermal degradation process during silk combustion is changed, and the flame retardant effect is achieved. The silk treated by the combination of the tannic acid and the metal salt has good flame retardant property and excellent washability.
The above-mentioned embodiments are merely preferred embodiments for fully illustrating the present invention, and the scope of the present invention is not limited thereto. The equivalent substitution or change made by the technical personnel in the technical field on the basis of the invention is all within the protection scope of the invention. The protection scope of the invention is subject to the claims.
Claims (6)
1. The method for preparing the flame-retardant silk is characterized by comprising the following steps of:
s1, immersing silk into a tannic acid solution with the pH value of 3-4, heating to 80-90 ℃, and carrying out heat preservation treatment;
and S2, immersing the silk processed in the step S1 into a metal salt solution of 2-6g/L, and heating to 50-70 ℃ for processing to obtain the flame-retardant silk.
2. The method for preparing flame-retardant silk according to claim 1, wherein the heat preservation treatment time in the step S1 is 45-75 min.
3. The method for preparing flame-retardant silk according to claim 1, wherein the treatment time at 50-70 ℃ in the step S2 is 20-40 min.
4. The method for preparing flame-retardant silk according to claim 1, wherein the tannin is used in an amount of 10-30% relative to the weight of the silk in step S1.
5. The method for preparing flame-retardant silk according to claim 1, wherein the metal salt is one or more of ferrous sulfate, ferric sulfate, titanium sulfate or calcium sulfate.
6. Flame-retardant silk prepared according to the method of any one of claims 1 to 5.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201811270759.6A CN109371660B (en) | 2018-10-29 | 2018-10-29 | Flame-retardant silk and preparation method and application thereof |
| PCT/CN2018/113686 WO2020087499A1 (en) | 2018-10-29 | 2018-11-02 | Flame retardant silk, preparation method therefor and use thereof |
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| CN201811270759.6A CN109371660B (en) | 2018-10-29 | 2018-10-29 | Flame-retardant silk and preparation method and application thereof |
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| CN109371660B true CN109371660B (en) | 2021-05-28 |
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| CN109371670B (en) * | 2018-10-29 | 2020-10-27 | 南通纺织丝绸产业技术研究院 | Flame-retardant silk and preparation method and application thereof |
| CN109457470A (en) * | 2018-11-16 | 2019-03-12 | 南通纺织丝绸产业技术研究院 | The flame-retardant silk and its preparation method and application prepared using flavones and metal salt |
| CN109837750B (en) * | 2019-03-06 | 2021-05-18 | 苏州大学 | Casein phosphopeptide-based silk durability flame-retardant finishing method and flame-retardant silk |
| CN110172823B (en) * | 2019-06-27 | 2020-10-30 | 四川大学 | Preparation method of formaldehyde-free washable flame-retardant fabric |
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| CN107245881A (en) * | 2017-07-13 | 2017-10-13 | 苏州大学 | Fire retarding treating liquid and the method that durable flame-retardant arrangement is carried out to silk fabric |
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| GB191415820A (en) * | 1914-07-02 | 1915-03-18 | Samuel Heap And Son Ltd | Improvements in Dyeing Artificial Silk. |
| CN1054413C (en) * | 1994-12-08 | 2000-07-12 | 浙江丝绸工学院 | Processing method for antisectic and deodorant textile material and its products |
| CN102140122A (en) * | 2011-01-25 | 2011-08-03 | 张维军 | Tannic acid metal salt, preparation method and application thereof |
| CN102767077B (en) * | 2012-07-06 | 2013-12-18 | 河南工程学院 | Dyeing method for soybean fibres and blended fabric of soybean fibres |
| CN108653741B (en) * | 2018-05-24 | 2021-06-25 | 华中科技大学同济医学院附属协和医院 | Metal organic coordination polymer coated natural sericin microsphere and preparation method and application thereof |
| CN108708163A (en) * | 2018-06-19 | 2018-10-26 | 如皋市万龙服装厂 | A kind of textile degerming method of simple process |
| CN109355902B (en) * | 2018-10-19 | 2020-03-10 | 南通纺织丝绸产业技术研究院 | Reactive flame retardant and method for carrying out durable flame-retardant finishing on protein fibers by using same |
| CN109371670B (en) * | 2018-10-29 | 2020-10-27 | 南通纺织丝绸产业技术研究院 | Flame-retardant silk and preparation method and application thereof |
| CN109281168B (en) * | 2018-10-31 | 2020-05-01 | 南通纺织丝绸产业技术研究院 | Soluble polyelectrolyte compound and method for flame-retardant finishing of protein fiber by using same |
| CN109457470A (en) * | 2018-11-16 | 2019-03-12 | 南通纺织丝绸产业技术研究院 | The flame-retardant silk and its preparation method and application prepared using flavones and metal salt |
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| CN107245881A (en) * | 2017-07-13 | 2017-10-13 | 苏州大学 | Fire retarding treating liquid and the method that durable flame-retardant arrangement is carried out to silk fabric |
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