CN109371660B - A kind of flame retardant silk and its preparation method and application - Google Patents
A kind of flame retardant silk and its preparation method and application Download PDFInfo
- Publication number
- 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
- Authority
- CN
- China
- Prior art keywords
- silk
- flame
- retardant
- flame retardant
- tannic acid
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
- RNFJDJUURJAICM-UHFFFAOYSA-N 2,2,4,4,6,6-hexaphenoxy-1,3,5-triaza-2$l^{5},4$l^{5},6$l^{5}-triphosphacyclohexa-1,3,5-triene Chemical compound N=1P(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP=1(OC=1C=CC=CC=1)OC1=CC=CC=C1 RNFJDJUURJAICM-UHFFFAOYSA-N 0.000 title claims abstract description 76
- 239000003063 flame retardant Substances 0.000 title claims abstract description 75
- 238000002360 preparation method Methods 0.000 title description 3
- 238000000034 method Methods 0.000 claims abstract description 37
- TUSDEZXZIZRFGC-UHFFFAOYSA-N 1-O-galloyl-3,6-(R)-HHDP-beta-D-glucose Natural products OC1C(O2)COC(=O)C3=CC(O)=C(O)C(O)=C3C3=C(O)C(O)=C(O)C=C3C(=O)OC1C(O)C2OC(=O)C1=CC(O)=C(O)C(O)=C1 TUSDEZXZIZRFGC-UHFFFAOYSA-N 0.000 claims abstract description 34
- 239000001263 FEMA 3042 Substances 0.000 claims abstract description 34
- LRBQNJMCXXYXIU-PPKXGCFTSA-N Penta-digallate-beta-D-glucose Natural products OC1=C(O)C(O)=CC(C(=O)OC=2C(=C(O)C=C(C=2)C(=O)OC[C@@H]2[C@H]([C@H](OC(=O)C=3C=C(OC(=O)C=4C=C(O)C(O)=C(O)C=4)C(O)=C(O)C=3)[C@@H](OC(=O)C=3C=C(OC(=O)C=4C=C(O)C(O)=C(O)C=4)C(O)=C(O)C=3)[C@H](OC(=O)C=3C=C(OC(=O)C=4C=C(O)C(O)=C(O)C=4)C(O)=C(O)C=3)O2)OC(=O)C=2C=C(OC(=O)C=3C=C(O)C(O)=C(O)C=3)C(O)=C(O)C=2)O)=C1 LRBQNJMCXXYXIU-PPKXGCFTSA-N 0.000 claims abstract description 34
- LRBQNJMCXXYXIU-NRMVVENXSA-N tannic acid Chemical compound OC1=C(O)C(O)=CC(C(=O)OC=2C(=C(O)C=C(C=2)C(=O)OC[C@@H]2[C@H]([C@H](OC(=O)C=3C=C(OC(=O)C=4C=C(O)C(O)=C(O)C=4)C(O)=C(O)C=3)[C@@H](OC(=O)C=3C=C(OC(=O)C=4C=C(O)C(O)=C(O)C=4)C(O)=C(O)C=3)[C@@H](OC(=O)C=3C=C(OC(=O)C=4C=C(O)C(O)=C(O)C=4)C(O)=C(O)C=3)O2)OC(=O)C=2C=C(OC(=O)C=3C=C(O)C(O)=C(O)C=3)C(O)=C(O)C=2)O)=C1 LRBQNJMCXXYXIU-NRMVVENXSA-N 0.000 claims abstract description 34
- 229940033123 tannic acid Drugs 0.000 claims abstract description 34
- 235000015523 tannic acid Nutrition 0.000 claims abstract description 34
- 229920002258 tannic acid Polymers 0.000 claims abstract description 34
- 239000000243 solution Substances 0.000 claims abstract description 14
- 229910052751 metal Inorganic materials 0.000 claims abstract description 10
- 239000002184 metal Substances 0.000 claims abstract description 10
- 238000010438 heat treatment Methods 0.000 claims abstract description 8
- 238000004321 preservation Methods 0.000 claims abstract description 5
- 238000012545 processing Methods 0.000 claims abstract description 5
- 239000012266 salt solution Substances 0.000 claims abstract description 3
- 235000003891 ferrous sulphate Nutrition 0.000 claims description 11
- 239000011790 ferrous sulphate Substances 0.000 claims description 11
- BAUYGSIQEAFULO-UHFFFAOYSA-L iron(2+) sulfate (anhydrous) Chemical compound [Fe+2].[O-]S([O-])(=O)=O BAUYGSIQEAFULO-UHFFFAOYSA-L 0.000 claims description 11
- 229910000359 iron(II) sulfate Inorganic materials 0.000 claims description 11
- OSGAYBCDTDRGGQ-UHFFFAOYSA-L calcium sulfate Chemical compound [Ca+2].[O-]S([O-])(=O)=O OSGAYBCDTDRGGQ-UHFFFAOYSA-L 0.000 claims description 10
- 150000003839 salts Chemical class 0.000 claims description 6
- RUTXIHLAWFEWGM-UHFFFAOYSA-H iron(3+) sulfate Chemical compound [Fe+3].[Fe+3].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O RUTXIHLAWFEWGM-UHFFFAOYSA-H 0.000 claims description 5
- 229910000360 iron(III) sulfate Inorganic materials 0.000 claims description 5
- DCKVFVYPWDKYDN-UHFFFAOYSA-L oxygen(2-);titanium(4+);sulfate Chemical compound [O-2].[Ti+4].[O-]S([O-])(=O)=O DCKVFVYPWDKYDN-UHFFFAOYSA-L 0.000 claims description 5
- 229910000348 titanium sulfate Inorganic materials 0.000 claims description 5
- 229920001864 tannin Polymers 0.000 claims 1
- 235000018553 tannin Nutrition 0.000 claims 1
- 239000001648 tannin Substances 0.000 claims 1
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 abstract description 12
- 229910052736 halogen Inorganic materials 0.000 abstract description 8
- 150000002367 halogens Chemical class 0.000 abstract description 8
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 abstract description 7
- 229910052698 phosphorus Inorganic materials 0.000 abstract description 7
- 239000011574 phosphorus Substances 0.000 abstract description 7
- 230000008569 process Effects 0.000 abstract description 7
- 229910052757 nitrogen Inorganic materials 0.000 abstract description 6
- 230000007613 environmental effect Effects 0.000 abstract description 5
- 238000004519 manufacturing process Methods 0.000 abstract description 4
- 238000003912 environmental pollution Methods 0.000 abstract description 3
- 238000005406 washing Methods 0.000 description 10
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 9
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 description 9
- 239000004744 fabric Substances 0.000 description 9
- 239000001301 oxygen Substances 0.000 description 9
- 229910052760 oxygen Inorganic materials 0.000 description 9
- 238000002485 combustion reaction Methods 0.000 description 7
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 7
- 230000000694 effects Effects 0.000 description 6
- 238000004140 cleaning Methods 0.000 description 5
- 239000004753 textile Substances 0.000 description 5
- 239000000835 fiber Substances 0.000 description 4
- 229910021645 metal ion Inorganic materials 0.000 description 4
- 238000002791 soaking Methods 0.000 description 4
- WSFSSNUMVMOOMR-UHFFFAOYSA-N Formaldehyde Chemical compound O=C WSFSSNUMVMOOMR-UHFFFAOYSA-N 0.000 description 3
- BNIILDVGGAEEIG-UHFFFAOYSA-L disodium hydrogen phosphate Chemical compound [Na+].[Na+].OP([O-])([O-])=O BNIILDVGGAEEIG-UHFFFAOYSA-L 0.000 description 3
- 238000001035 drying Methods 0.000 description 3
- 238000000643 oven drying Methods 0.000 description 3
- 239000008055 phosphate buffer solution Substances 0.000 description 3
- 238000003756 stirring Methods 0.000 description 3
- 230000002378 acidificating effect Effects 0.000 description 2
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 description 2
- 238000006731 degradation reaction Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 102000004169 proteins and genes Human genes 0.000 description 2
- 108090000623 proteins and genes Proteins 0.000 description 2
- 238000009987 spinning Methods 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- 229920000742 Cotton Polymers 0.000 description 1
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 1
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 description 1
- YUWBVKYVJWNVLE-UHFFFAOYSA-N [N].[P] Chemical compound [N].[P] YUWBVKYVJWNVLE-UHFFFAOYSA-N 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229910021538 borax Inorganic materials 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 238000007598 dipping method Methods 0.000 description 1
- 238000005108 dry cleaning Methods 0.000 description 1
- 238000004043 dyeing Methods 0.000 description 1
- 238000012851 eutrophication Methods 0.000 description 1
- 238000007730 finishing process Methods 0.000 description 1
- 230000036449 good health Effects 0.000 description 1
- 239000002932 luster Substances 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 229930014626 natural product Natural products 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 238000007639 printing Methods 0.000 description 1
- 239000000779 smoke Substances 0.000 description 1
- 239000004328 sodium tetraborate Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 238000009988 textile finishing Methods 0.000 description 1
- 229910052719 titanium Inorganic materials 0.000 description 1
- 239000010936 titanium Substances 0.000 description 1
- 239000002341 toxic gas Substances 0.000 description 1
- 231100000419 toxicity Toxicity 0.000 description 1
- 230000001988 toxicity Effects 0.000 description 1
- 210000002268 wool Anatomy 0.000 description 1
- 229910052726 zirconium Inorganic materials 0.000 description 1
Classifications
-
- 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
-
- 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
-
- 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
-
- 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
Landscapes
- Engineering & Computer Science (AREA)
- Textile Engineering (AREA)
- Treatments For Attaching Organic Compounds To Fibrous Goods (AREA)
- Chemical Or Physical Treatment Of Fibers (AREA)
Abstract
本发明公开了一种制备阻燃蚕丝的方法，包括以下步骤：将蚕丝浸入pH值为3‑4的单宁酸溶液中，升温至80‑90℃进行保温处理；将经过处理后的蚕丝浸入至2‑6g/L的金属盐溶液中，并升温至50‑70℃进行处理，得到阻燃蚕丝。本发明的方法在不添加含有传统氮、磷、卤族元素阻燃剂的情况下赋予蚕丝良好的阻燃性能，并且能够避免因使用传统阻燃剂而带来的在阻燃蚕丝生产和使用过程中以及及阻燃蚕丝被废弃后氮、磷、卤族元素带来的环境污染问题。该方法具有环保、高效、简单易行的优点。The invention discloses a method for preparing flame-retardant silk, comprising the following steps: immersing the silk in a tannic acid solution with a pH value of 3-4, heating up to 80-90° C. for heat preservation treatment; immersing the treated silk in a tannic acid solution into a metal salt solution of 2-6g/L, and the temperature is raised to 50-70°C for processing to obtain flame-retardant silk. The method of the invention imparts good flame retardant properties to silk without adding flame retardants containing traditional nitrogen, phosphorus and halogen elements, and can avoid the production and use of flame retardant silk caused by the use of traditional flame retardants. During the process and the environmental pollution caused by nitrogen, phosphorus and halogen elements after the flame retardant silk is discarded. The method has the advantages of environmental protection, high efficiency and simplicity.
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.
Priority Applications (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811270759.6A CN109371660B (en) | 2018-10-29 | 2018-10-29 | A kind of flame retardant silk and its preparation method and application |
| PCT/CN2018/113686 WO2020087499A1 (en) | 2018-10-29 | 2018-11-02 | Flame retardant silk, preparation method therefor and use thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811270759.6A CN109371660B (en) | 2018-10-29 | 2018-10-29 | A kind of flame retardant silk and its preparation method and application |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN109371660A CN109371660A (en) | 2019-02-22 |
| CN109371660B true CN109371660B (en) | 2021-05-28 |
Family
ID=65390038
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201811270759.6A Active CN109371660B (en) | 2018-10-29 | 2018-10-29 | A kind of flame retardant silk and its preparation method and application |
Country Status (2)
| Country | Link |
|---|---|
| CN (1) | CN109371660B (en) |
| WO (1) | WO2020087499A1 (en) |
Families Citing this family (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 its preparation method and application |
| 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 | Durable flame retardant finishing method of silk based on casein phosphopeptide and flame retardant silk |
| CN110172823B (en) * | 2019-06-27 | 2020-10-30 | 四川大学 | A kind of preparation method of formaldehyde-free washing-resistant flame-retardant fabric |
| CN116289255A (en) * | 2023-03-29 | 2023-06-23 | 厦门求特新材料有限公司 | A kind of anti-aging preparation process of heavy-duty webbing |
| CN119162825A (en) * | 2024-10-17 | 2024-12-20 | 广州云照汉唐国际文化传播有限公司 | Flame-retardant silk fiber material and flame-retardant silk fabric and preparation method thereof |
| CN121610987A (en) * | 2024-12-16 | 2026-03-06 | 江苏鑫缘丝绸科技有限公司 | Flame-retardant silk fabric with PEI-GA/Me composite coating |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
Family Cites Families (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 | A kind of natural sericin microspheres encapsulated by metal-organic coordination polymer and its preparation method and application |
| 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 its preparation method and application |
| CN109281168B (en) * | 2018-10-31 | 2020-05-01 | 南通纺织丝绸产业技术研究院 | Soluble polyelectrolyte composite and method for flame retardant finishing of protein fiber |
| 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 |
-
2018
- 2018-10-29 CN CN201811270759.6A patent/CN109371660B/en active Active
- 2018-11-02 WO PCT/CN2018/113686 patent/WO2020087499A1/en not_active Ceased
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
Also Published As
| Publication number | Publication date |
|---|---|
| CN109371660A (en) | 2019-02-22 |
| WO2020087499A1 (en) | 2020-05-07 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN109371660B (en) | A kind of flame retardant silk and its preparation method and application | |
| CN109183408B (en) | Layer-by-layer self-assembled flame-retardant cotton fabric and preparation method thereof | |
| CN109281168B (en) | Soluble polyelectrolyte composite and method for flame retardant finishing of protein fiber | |
| CN103321044B (en) | A kind of flame-retardant pure silk and preparation method thereof | |
| WO2020097981A1 (en) | Flame-retardant silk prepared from flavone and metal salt, preparation method therefor, and application thereof | |
| CN106544867B (en) | Colored flame-retardant polyester-cotton fabric and preparation method thereof | |
| CN107245881B (en) | Flame-retardant finishing solution and method for durable flame-retardant finishing of silk fabrics | |
| CN110172823B (en) | A kind of preparation method of formaldehyde-free washing-resistant flame-retardant fabric | |
| CN112227067A (en) | Preparation process of non-soaked antibacterial deodorant cotton | |
| CN103710993B (en) | A kind of preparation technology of the silver-colored silicon complex antimicrobials with permanent antibacterial action | |
| CN102433762B (en) | Method for preparing flame retardant down feathers | |
| CN110747630A (en) | Waterproof flame-retardant textile and preparation method thereof | |
| CN111423463A (en) | Preparation method and application of reactive boron-containing flame retardant | |
| CN109371670B (en) | Flame retardant silk and its preparation method and application | |
| CN102660869A (en) | Method for preparing inflaming-retarding wool fabric and inflaming-retarding working solution | |
| CN114687201B (en) | Preparation method of honeysuckle dyed antibacterial textile and product thereof | |
| CN103952916B (en) | A kind of preparation method of flame-retardant acrylic fibre | |
| CN111074549A (en) | Multifunctional after-finishing process of pure cotton fabric | |
| CN112127153A (en) | Antibacterial and deodorant textile and preparation method thereof | |
| CN119102103A (en) | Preparation method of halogen-free nitrogen-phosphorus-silicon-containing flexible flame-retardant cotton fabric | |
| CN111074597A (en) | Multifunctional after-finishing process of polyester-cotton fabric | |
| CN111851060A (en) | Preparation method of nano-silver antibacterial natural plush fiber product | |
| CN109837750B (en) | Durable flame retardant finishing method of silk based on casein phosphopeptide and flame retardant silk | |
| CN119686109B (en) | A flame-retardant silk fabric and its preparation method | |
| CN117127404B (en) | A composite fabric modifier and a method for co-modifying cotton fabrics thereof |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |