CN109826011B - A kind of alginic acid derivative halogen-free flame retardant fiber cloth and preparation method thereof - Google Patents
A kind of alginic acid derivative halogen-free flame retardant fiber cloth and preparation method thereof Download PDFInfo
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- 239000003063 flame retardant Substances 0.000 title claims description 88
- 239000004744 fabric Substances 0.000 title claims description 85
- 235000010443 alginic acid Nutrition 0.000 title claims description 59
- 229920000615 alginic acid Polymers 0.000 title claims description 59
- 239000000835 fiber Substances 0.000 title claims description 59
- 150000004781 alginic acids Chemical class 0.000 title claims description 55
- 239000000783 alginic acid Substances 0.000 title claims description 54
- 229960001126 alginic acid Drugs 0.000 title claims description 54
- DXZMANYCMVCPIM-UHFFFAOYSA-L zinc;diethylphosphinate Chemical compound [Zn+2].CCP([O-])(=O)CC.CCP([O-])(=O)CC DXZMANYCMVCPIM-UHFFFAOYSA-L 0.000 title claims description 34
- 238000002360 preparation method Methods 0.000 title claims description 13
- 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 claims description 51
- 239000006185 dispersion Substances 0.000 claims description 21
- 238000003756 stirring Methods 0.000 claims description 18
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 18
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 16
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 15
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 claims description 12
- 239000002904 solvent Substances 0.000 claims description 9
- IMQLKJBTEOYOSI-GPIVLXJGSA-N Inositol-hexakisphosphate Chemical compound OP(O)(=O)O[C@H]1[C@H](OP(O)(O)=O)[C@@H](OP(O)(O)=O)[C@H](OP(O)(O)=O)[C@H](OP(O)(O)=O)[C@@H]1OP(O)(O)=O IMQLKJBTEOYOSI-GPIVLXJGSA-N 0.000 claims description 8
- ZXEKIIBDNHEJCQ-UHFFFAOYSA-N isobutanol Chemical compound CC(C)CO ZXEKIIBDNHEJCQ-UHFFFAOYSA-N 0.000 claims description 8
- 235000002949 phytic acid Nutrition 0.000 claims description 8
- OFBQJSOFQDEBGM-UHFFFAOYSA-N Pentane Chemical compound CCCCC OFBQJSOFQDEBGM-UHFFFAOYSA-N 0.000 claims description 6
- 229920002994 synthetic fiber Polymers 0.000 claims description 6
- 239000012209 synthetic fiber Substances 0.000 claims description 6
- FHVDTGUDJYJELY-UHFFFAOYSA-N 6-{[2-carboxy-4,5-dihydroxy-6-(phosphanyloxy)oxan-3-yl]oxy}-4,5-dihydroxy-3-phosphanyloxane-2-carboxylic acid Chemical compound O1C(C(O)=O)C(P)C(O)C(O)C1OC1C(C(O)=O)OC(OP)C(O)C1O FHVDTGUDJYJELY-UHFFFAOYSA-N 0.000 claims description 5
- 229920000742 Cotton Polymers 0.000 claims description 5
- 229920000388 Polyphosphate Polymers 0.000 claims description 5
- 229940072056 alginate Drugs 0.000 claims description 5
- WNROFYMDJYEPJX-UHFFFAOYSA-K aluminium hydroxide Chemical compound [OH-].[OH-].[OH-].[Al+3] WNROFYMDJYEPJX-UHFFFAOYSA-K 0.000 claims description 5
- 239000001205 polyphosphate Substances 0.000 claims description 5
- 235000011176 polyphosphates Nutrition 0.000 claims description 5
- 229920000137 polyphosphoric acid Polymers 0.000 claims description 5
- XZZNDPSIHUTMOC-UHFFFAOYSA-N triphenyl phosphate Chemical compound C=1C=CC=CC=1OP(OC=1C=CC=CC=1)(=O)OC1=CC=CC=C1 XZZNDPSIHUTMOC-UHFFFAOYSA-N 0.000 claims description 5
- BIKXLKXABVUSMH-UHFFFAOYSA-N trizinc;diborate Chemical compound [Zn+2].[Zn+2].[Zn+2].[O-]B([O-])[O-].[O-]B([O-])[O-] BIKXLKXABVUSMH-UHFFFAOYSA-N 0.000 claims description 5
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 claims description 4
- IMQLKJBTEOYOSI-UHFFFAOYSA-N Phytic acid Natural products OP(O)(=O)OC1C(OP(O)(O)=O)C(OP(O)(O)=O)C(OP(O)(O)=O)C(OP(O)(O)=O)C1OP(O)(O)=O IMQLKJBTEOYOSI-UHFFFAOYSA-N 0.000 claims description 4
- 229920002334 Spandex Polymers 0.000 claims description 4
- 229910052698 phosphorus Inorganic materials 0.000 claims description 4
- 239000011574 phosphorus Substances 0.000 claims description 4
- 239000000467 phytic acid Substances 0.000 claims description 4
- 229940068041 phytic acid Drugs 0.000 claims description 4
- 239000004759 spandex Substances 0.000 claims description 4
- XDTMQSROBMDMFD-UHFFFAOYSA-N Cyclohexane Chemical compound C1CCCCC1 XDTMQSROBMDMFD-UHFFFAOYSA-N 0.000 claims description 3
- 239000004952 Polyamide Substances 0.000 claims description 3
- 229920002521 macromolecule Polymers 0.000 claims description 3
- 229920002647 polyamide Polymers 0.000 claims description 3
- 229920002978 Vinylon Polymers 0.000 claims 2
- NIXOWILDQLNWCW-UHFFFAOYSA-N acrylic acid group Chemical group C(C=C)(=O)O NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 claims 1
- 229920000728 polyester Polymers 0.000 claims 1
- 239000007788 liquid Substances 0.000 description 19
- 238000001035 drying Methods 0.000 description 10
- 238000002791 soaking Methods 0.000 description 6
- 238000000034 method Methods 0.000 description 5
- 239000011259 mixed solution Substances 0.000 description 5
- 229910052710 silicon Inorganic materials 0.000 description 5
- 239000010703 silicon Substances 0.000 description 5
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 description 4
- 238000002485 combustion reaction Methods 0.000 description 4
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 3
- 229920004933 Terylene® Polymers 0.000 description 3
- 239000012153 distilled water Substances 0.000 description 3
- 238000010981 drying operation Methods 0.000 description 3
- 239000005020 polyethylene terephthalate Substances 0.000 description 3
- 229920002972 Acrylic fiber Polymers 0.000 description 2
- 229920006052 Chinlon® Polymers 0.000 description 2
- PIICEJLVQHRZGT-UHFFFAOYSA-N Ethylenediamine Chemical class NCCN PIICEJLVQHRZGT-UHFFFAOYSA-N 0.000 description 2
- 239000004677 Nylon Substances 0.000 description 2
- 229920002302 Nylon 6,6 Polymers 0.000 description 2
- 229910019142 PO4 Inorganic materials 0.000 description 2
- 229910000147 aluminium phosphate Inorganic materials 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 229920001778 nylon Polymers 0.000 description 2
- 235000021317 phosphate Nutrition 0.000 description 2
- 239000010452 phosphate Substances 0.000 description 2
- XHXFXVLFKHQFAL-UHFFFAOYSA-N phosphoryl trichloride Chemical compound ClP(Cl)(Cl)=O XHXFXVLFKHQFAL-UHFFFAOYSA-N 0.000 description 2
- 238000006116 polymerization reaction Methods 0.000 description 2
- 239000000243 solution Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 238000006467 substitution reaction Methods 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- 239000004753 textile Substances 0.000 description 2
- 229920002554 vinyl polymer Polymers 0.000 description 2
- AEMOLEFTQBMNLQ-AZLKCVHYSA-N (2r,3s,4s,5s,6r)-3,4,5,6-tetrahydroxyoxane-2-carboxylic acid Chemical compound O[C@@H]1O[C@@H](C(O)=O)[C@@H](O)[C@H](O)[C@@H]1O AEMOLEFTQBMNLQ-AZLKCVHYSA-N 0.000 description 1
- BSYJHYLAMMJNRC-UHFFFAOYSA-N 2,4,4-trimethylpentan-2-ol Chemical compound CC(C)(C)CC(C)(C)O BSYJHYLAMMJNRC-UHFFFAOYSA-N 0.000 description 1
- WMYINDVYGQKYMI-UHFFFAOYSA-N 2-[2,2-bis(hydroxymethyl)butoxymethyl]-2-ethylpropane-1,3-diol Chemical compound CCC(CO)(CO)COCC(CC)(CO)CO WMYINDVYGQKYMI-UHFFFAOYSA-N 0.000 description 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- 239000012752 auxiliary agent Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000000903 blocking effect Effects 0.000 description 1
- 238000003763 carbonization Methods 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 238000009833 condensation Methods 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 210000000805 cytoplasm Anatomy 0.000 description 1
- AEMOLEFTQBMNLQ-YBSDWZGDSA-N d-mannuronic acid Chemical compound O[C@@H]1O[C@@H](C(O)=O)[C@H](O)[C@@H](O)[C@H]1O AEMOLEFTQBMNLQ-YBSDWZGDSA-N 0.000 description 1
- 230000018044 dehydration Effects 0.000 description 1
- 238000006297 dehydration reaction Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000007598 dipping method Methods 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 238000004043 dyeing Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 238000005886 esterification reaction Methods 0.000 description 1
- 150000002148 esters Chemical class 0.000 description 1
- 238000011156 evaluation Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- -1 flame retardant ditrimethylolpropane phosphate ester ethylenediamine salt Chemical class 0.000 description 1
- VOZRXNHHFUQHIL-UHFFFAOYSA-N glycidyl methacrylate Chemical compound CC(=C)C(=O)OCC1CO1 VOZRXNHHFUQHIL-UHFFFAOYSA-N 0.000 description 1
- 229910052736 halogen Inorganic materials 0.000 description 1
- 150000002367 halogens Chemical class 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
- 239000003999 initiator Substances 0.000 description 1
- 229920005684 linear copolymer Polymers 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000002715 modification method Methods 0.000 description 1
- 239000012466 permeate Substances 0.000 description 1
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 description 1
- 238000007639 printing Methods 0.000 description 1
- 239000011241 protective layer Substances 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 238000003892 spreading Methods 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
Landscapes
- Treatments For Attaching Organic Compounds To Fibrous Goods (AREA)
- Chemical Or Physical Treatment Of Fibers (AREA)
Abstract
本发明公开了一种海藻酸衍生物无卤阻燃纤维布及其制备方法，涉及阻燃织物技术领域。一种海藻酸衍生物无卤阻燃纤维布，包括海藻酸衍生物、无卤阻燃剂和纤维布，所述海藻酸衍生物是一种磷、硅海藻酸盐自聚型柔性大分子。在纤维布浸渍过程中，海藻酸衍生物吸附于纤维布表面裸露在外的硅羟基在后加热过程中会与海藻酸衍生物发生酯化反应以及硅羟基脱水自缩合实现大分子化，从而形成具有交联结构的柔性高分子阻燃剂薄膜包覆于织物纤维表面，获得一种半永久性的阻燃纤维布，无卤阻燃剂进一步增大纤维布的阻燃性能，这种阻燃纤维布阻燃性能优异且不产生熔滴。The invention discloses an alginic acid derivative halogen-free flame-retardant fiber cloth and a preparation method thereof, and relates to the technical field of flame-retardant fabrics. An alginic acid derivative halogen-free flame retardant fiber cloth, comprising alginic acid derivative, halogen-free flame retardant and fiber cloth, the alginic acid derivative is a kind of phosphorus, silicic alginate self-polymerization flexible macromolecule. During the impregnation process of the fiber cloth, the alginic acid derivatives adsorbed on the exposed silanols on the surface of the fiber cloth will undergo esterification reaction with the alginic acid derivatives and dehydration and self-condensation of the silanols during the post-heating process to achieve macromolecularization, thereby forming a A flexible polymer flame retardant film with a cross-linked structure is coated on the surface of the fabric fiber to obtain a semi-permanent flame retardant fiber cloth. The halogen-free flame retardant further increases the flame retardant performance of the fiber cloth. This flame retardant fiber cloth Excellent flame retardant properties and no droplets.
Description
Technical Field
The invention relates to the technical field of flame-retardant fabrics, in particular to alginic acid derivative halogen-free flame-retardant fiber cloth and a preparation method thereof.
Background
The fiber fabric has wide application in daily life, military, construction, biology, medicine and other aspects. However, since untreated fiber cloth is generally flammable, it is easy to cause fire, and causes huge economic loss and casualties. Endowing the textile with better flame retardance has become a necessary trend of development, and various countries gradually come out of law and put forward corresponding flame retardance requirements on the flame retardance of the textile.
The method introduces a microwave grafting modification method in the flame retardant property of microwave grafting modified nylon 66 fabric (Beijing university of chemical industry, Nature science edition, 2016,43(2):19-26), which comprises the steps of sequentially grafting Glycidyl Methacrylate (GMA) and 9, 10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide (DOPO) onto the surface of the nylon 66 fabric, and carrying out grafting reaction under the microwave power of 500W by taking KPS as an initiator. After grafting, the fabric char-forming performance is enhanced, the flame retardant performance is improved, but the preparation process is complex and the grafting rate is low.
Li Xiang et al in "application research on multifunctional phosphate ester ethylenediamine salt flame retardant on nylon fabric" (Li Xiang, Ding bin, Haofenling, etc. printing and dyeing auxiliary agent, 2015(1):45-48) with ditrimethylolpropane, phosphorus oxychloride and ethylenediamine as raw materials, synthesize multifunctional flame retardant ditrimethylolpropane phosphate ester ethylenediamine salt, and finish the nylon fabric with it, the result shows, the fabric flame retardant effect after finishing is obvious, but this flame retardant has the disadvantages of more complicated preparation process, higher fabric treatment temperature.
As can be seen from the above, most of the existing flame-retardant fabrics are modified by flame retardants to have good flame-retardant performance, but the process for preparing the flame-retardant fabrics by using the flame retardants is complex, the halogen-containing or fabric treatment temperature is too high, certain harm is caused to the environment, the energy consumption is high, and the flame-retardant fabrics are not suitable for industrial application.
Alginate is a linear copolymer salt formed by 1,4 bonding of alpha-L-mannuronic acid and alpha-L-guluronic acid. In nature, alginate is present in the cytoplasm and is a biodegradable material. In recent years, alginic acid substances are applied to various fields such as biological dressings, biological scaffolds, green flame retardance and the like, have good biocompatibility and flame retardance, are environment-friendly materials, and have great application prospects.
Disclosure of Invention
Aiming at the problems, the invention provides the alginic acid derivative halogen-free flame retardant fiber cloth and the preparation method thereof, the preparation method is simple and environment-friendly, and the obtained alginic acid derivative halogen-free flame retardant fiber cloth has excellent flame retardant property. The technical scheme adopted by the invention is as follows:
the alginic acid derivative is a self-polymerization type flexible macromolecule of phosphorus and silicon alginate.
Further, the alginic acid derivative has a structure of:
further, the halogen-free flame retardant comprises at least one of aluminum hydroxide, polyphosphoric acid, polyphosphate, triphenyl phosphate, phytic acid, phytate and zinc borate.
Further, the mass ratio of the total mass of the alginic acid derivative and the halogen-free flame retardant to the fiber cloth is 0.05-0.95: 1.
further, the fiber cloth is natural fiber cloth or synthetic fiber cloth.
Further, the natural fiber cloth is cotton fiber cloth or silk.
Further, the synthetic fiber cloth is one of terylene, chinlon, acrylic fiber, polyvinyl fiber or spandex.
Further, the preparation method of the alginic acid derivative halogen-free flame retardant fiber cloth comprises the following steps:
s1, adding the alginic acid derivative with the formula amount into a solvent at room temperature, stirring for 10-20 min, adding the halogen-free flame retardant with the formula amount, and continuously stirring for 10-15 min to obtain a flame retardant dispersion liquid;
s2, soaking the fiber cloth with the formula amount into the flame retardant dispersion liquid in the step S1, standing for 1-30 min, taking out, controlling to be dry until no water drops, and drying at 40-80 ℃ for 2-8 h to obtain dry fiber cloth;
and S3, repeating the step S20-4 times to obtain the alginic acid derivative halogen-free flame-retardant fiber cloth.
Further, in the step S1, the solvent is at least one of water, methanol, ethanol, isobutanol, pentane, hexane, and cyclohexane.
Further, in the step S1, the mass ratio of the total mass of the alginic acid derivative and the halogen-free flame retardant to the solvent is 0.01 to 0.35: 1.
due to the adoption of the technical scheme, the invention has the beneficial effects that:
in the dipping process, alginic acid derivatives are adsorbed on the surface of the fiber cloth, and the exposed silicon hydroxyl can be subjected to esterification reaction with the alginic acid derivatives and silicon hydroxyl is subjected to dehydration and self-condensation in the post-heating process to realize the macromolecularization, so that a flexible high-molecular flame retardant film with a cross-linked structure is formed and coated on the surface of the fabric fiber, and the semi-permanent flame retardant fiber cloth is obtained. The flame-retardant fiber cloth can generate phosphoric acid to carbonize a fiber cloth substrate in the combustion process, and the phosphoric acid can further generate phosphorus-containing free radicals, can capture hydrogen free radicals and hydroxyl free radicals generated by combustion, and plays a role in blocking a fire source to achieve the purpose of flame retardance. Meanwhile, alginic acid part and silicon-containing group in the flame retardant can form a carbonization protective layer in the flame retardant process, isolate the heat mass from spreading, protect the basal body from the flame; in addition, the added halogen-free flame retardant can permeate and be adsorbed on the surface of the fiber cloth in the coating process, and the halogen-free flame retardant and the alginic acid derivative form flame-retardant fiber cloth together, so that the generation of molten drops is further prevented, and the flame retardant property of the fiber cloth is enhanced. The preparation method of the alginic acid derivative halogen-free flame-retardant fiber cloth is simple and is suitable for industrial application.
Detailed Description
The present invention will be described in detail with reference to specific embodiments below:
the alginic acid derivative is a self-polymerization type flexible macromolecule of phosphorus and silicon alginate.
Further, the alginic acid derivative has a structure of:
further, the halogen-free flame retardant comprises at least one of aluminum hydroxide, polyphosphoric acid, polyphosphate, triphenyl phosphate, phytic acid, phytate and zinc borate.
Further, the mass ratio of the total mass of the alginic acid derivative and the halogen-free flame retardant to the fiber cloth is 0.05-0.95: 1.
further, the fiber cloth is natural fiber cloth or synthetic fiber cloth.
Further, the natural fiber cloth is cotton fiber cloth or silk.
Further, the synthetic fiber cloth is one of terylene, chinlon, acrylic fiber, polyvinyl fiber or spandex.
Further, the preparation method of the alginic acid derivative halogen-free flame retardant fiber cloth comprises the following steps:
s1, adding the alginic acid derivative with the formula amount into a solvent at room temperature, stirring for 10-20 min, adding the halogen-free flame retardant with the formula amount, and continuously stirring for 10-15 min to obtain a flame retardant dispersion liquid;
s2, soaking the fiber cloth with the formula amount into the flame retardant dispersion liquid in the step S1, standing for 1-30 min, taking out, controlling to be dry until no water drops, and drying at 40-80 ℃ for 2-8 h to obtain dry fiber cloth;
and S3, repeating the step S20-4 times to obtain the alginic acid derivative halogen-free flame-retardant fiber cloth.
Further, in the step S1, the solvent is at least one of water, methanol, ethanol, isobutanol, pentane, hexane, and cyclohexane.
Further, in the step S1, the mass ratio of the total mass of the alginic acid derivative and the halogen-free flame retardant to the solvent is 0.01 to 0.35: 1.
the embodiments of the present invention can be obtained by different substitutions in specific ranges based on the above technical solutions, and therefore, the following embodiments are only preferred embodiments of the embodiments, and any technical substitutions made by the above technical solutions are within the protection scope of the present invention.
Example 1
Adding 5g of alginic acid derivative into 100g of a 1:1 (volume ratio) mixed solution of distilled water and ethanol, stirring and dispersing for 10min, adding 2g of triphenyl phosphate and 2g of zinc borate, and continuously stirring and dispersing for 10min to obtain a flame retardant dispersion liquid; 20g of 30 x 30cm polyamide fabric is immersed into the flame retardant dispersion liquid for 3min, taken out and dried until no water drops, dried at 40 ℃ for 8h, immersed into the flame retardant dispersion liquid again for 3min, taken out and dried until no water drops, and dried at 40 ℃ for 8h to obtain the alginic acid derivative halogen-free flame retardant fiber fabric.
Example 2
Adding 10g of alginic acid derivative into 100g of a 1:1:1 (volume ratio) mixed solution of distilled water, methanol and ethanol, stirring and dispersing for 15min, adding 5g of phytic acid and 5g of aluminum hydroxide, and continuously stirring and dispersing for 10min to obtain a flame retardant dispersion liquid; and (3) soaking 20g of 30 x 30cm spandex cloth in the flame retardant dispersion liquid for 5min, taking out, drying until no water drops, drying at 50 ℃ for 6h, and repeating the soaking-drying operation for 4 times to obtain the alginic acid derivative halogen-free flame retardant fiber cloth.
Example 3
Adding 20g of alginic acid derivative into 100g of ethanol, stirring and dispersing for 20min, then stirring and dispersing 5g of polyphosphoric acid and 10g of polyphosphate for 15min to obtain a flame retardant dispersion liquid; and (3) soaking 20g of 30 x 30cm cotton fiber cloth in the flame retardant dispersion liquid for 5min, taking out, drying until no water drops, drying at 60 ℃ for 4h, and repeating the soaking-drying operation for 3 times to obtain the alginic acid derivative halogen-free flame retardant fiber cloth.
Example 4
Adding 0.5g alginic acid derivative into 100g mixed solution of ethanol and isobutanol 1:1 (volume ratio), stirring and dispersing for 20min, adding 0.2g phytate and 0.3g aluminum hydroxide, and continuing stirring and dispersing for 15min to obtain flame retardant dispersion liquid; and (3) soaking 20g of 30 x 30cm cotton fiber cloth into the flame retardant dispersion liquid for 10min, taking out, drying until no water drops, and drying at 80 ℃ for 2h to obtain the alginic acid derivative halogen-free flame retardant fiber cloth.
Example 5
Adding 10g of alginic acid derivative into 100g of a mixed solution of methanol and hexane in a volume ratio of 1:1, stirring and dispersing for 20min, adding 5g of polyphosphoric acid and 4g of polyphosphate, and continuously stirring and dispersing for 10min to obtain a flame retardant dispersion liquid; soaking 20g of 30 x 30cm terylene cloth in the flame retardant dispersion liquid for 5min, taking out, drying until no water drops, drying at 40 ℃ for 4h, and repeating the soaking-drying operation for 3 times to obtain the alginic acid derivative halogen-free flame retardant fiber cloth.
Example 6
Adding 6g of alginic acid derivative into 100g of a 1:1 (volume ratio) mixed solution of distilled water and ethanol, stirring and dispersing for 10min, adding 2g of triphenyl phosphate and 3g of zinc borate, and continuously stirring and dispersing for 15min to obtain a flame retardant dispersion liquid; 20g of 30 × 30cm polyamide fabric is immersed into the flame retardant dispersion liquid for 1min, taken out and dried until no water drops, dried for 2h at 40 ℃, immersed into the flame retardant dispersion liquid again for 10min, taken out and dried until no water drops, dried for 2h at 40 ℃, immersed into the flame retardant dispersion liquid again for 30min, taken out and dried until no water drops, and dried for 6h at 40 ℃ to obtain the alginic acid derivative halogen-free flame retardant fiber cloth.
Vertical combustion experiments were performed according to GBT 5455-1997 standard, with standard ratings:
level B1: a) the damage length is less than or equal to 150 mm; b) the burning time is less than or equal to 5 s; c) smoldering time is less than or equal to 5 s;
level B2: a) the damage length is less than or equal to 200 mm; b) the burning time is less than or equal to 15 s; c) the smoldering time is less than or equal to 10 s.
The test method comprises the following steps: measuring from a position which is far away from the cloth edge 1/10 in width, taking 15 samples in the warp direction and the weft direction respectively, wherein the sample size is as follows: 30 x 80 cm; 15 samples are respectively taken in the warp direction and the weft direction, the height of combustion flame is controlled to be 40 +/-2 mm, and the ignition time is as follows: 12 s.
The instrument model is adopted: vertical flame retardant tester HK-HVR.
The test results are shown in table 1 below:
TABLE 1 evaluation of alginic acid derivatives for halogen-free flame-retardant fiber cloth
As can be seen from the table, the alginic acid derivative halogen-free flame retardant fiber cloth has excellent flame retardant property, has no smoldering phenomenon in a flame retardant test, is self-extinguished after leaving fire, does not produce molten drops, and has superior performance compared with the commercially available sample 1.
The invention is not limited to the foregoing embodiments. The invention extends to any novel feature or any novel combination of features disclosed in this specification and any novel method or process steps or any novel combination of features disclosed.
Claims (9)
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811532380.8A CN109826011B (en) | 2018-12-14 | 2018-12-14 | A kind of alginic acid derivative halogen-free flame retardant fiber cloth and preparation method thereof |
Applications Claiming Priority (1)
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