CN111074544B - Preparation method and application of magnalium hydrotalcite flame-retardant modified jute fabric with different anion intercalation - Google Patents
Preparation method and application of magnalium hydrotalcite flame-retardant modified jute fabric with different anion intercalation Download PDFInfo
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- 240000000491 Corchorus aestuans Species 0.000 title claims abstract description 132
- 235000011777 Corchorus aestuans Nutrition 0.000 title claims abstract description 132
- 235000010862 Corchorus capsularis Nutrition 0.000 title claims abstract description 132
- 239000004744 fabric Substances 0.000 title claims abstract description 126
- 239000003063 flame retardant Substances 0.000 title claims abstract description 59
- 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 57
- 150000001450 anions Chemical class 0.000 title claims abstract description 37
- GDVKFRBCXAPAQJ-UHFFFAOYSA-A dialuminum;hexamagnesium;carbonate;hexadecahydroxide Chemical compound [OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[Mg+2].[Mg+2].[Mg+2].[Mg+2].[Mg+2].[Mg+2].[Al+3].[Al+3].[O-]C([O-])=O GDVKFRBCXAPAQJ-UHFFFAOYSA-A 0.000 title claims abstract description 37
- 229960001545 hydrotalcite Drugs 0.000 title claims abstract description 37
- 229910001701 hydrotalcite Inorganic materials 0.000 title claims abstract description 37
- 238000002360 preparation method Methods 0.000 title claims abstract description 28
- 238000009830 intercalation Methods 0.000 title claims abstract description 21
- 230000002687 intercalation Effects 0.000 title claims abstract description 13
- 229910001051 Magnalium Inorganic materials 0.000 title claims description 27
- SNAAJJQQZSMGQD-UHFFFAOYSA-N aluminum magnesium Chemical compound [Mg].[Al] SNAAJJQQZSMGQD-UHFFFAOYSA-N 0.000 claims abstract description 38
- 238000001035 drying Methods 0.000 claims abstract description 37
- 238000000034 method Methods 0.000 claims abstract description 31
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- 239000000243 solution Substances 0.000 claims description 59
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 54
- 238000001354 calcination Methods 0.000 claims description 24
- 239000000843 powder Substances 0.000 claims description 17
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 14
- 238000010438 heat treatment Methods 0.000 claims description 13
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 12
- 150000002500 ions Chemical class 0.000 claims description 11
- 239000011259 mixed solution Substances 0.000 claims description 11
- 230000032683 aging Effects 0.000 claims description 9
- VSCWAEJMTAWNJL-UHFFFAOYSA-K aluminium chloride Substances Cl[Al](Cl)Cl VSCWAEJMTAWNJL-UHFFFAOYSA-K 0.000 claims description 9
- 238000001816 cooling Methods 0.000 claims description 9
- 239000000706 filtrate Substances 0.000 claims description 9
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- 239000007787 solid Substances 0.000 claims description 9
- 239000000463 material Substances 0.000 claims description 7
- MOTZDAYCYVMXPC-UHFFFAOYSA-N dodecyl hydrogen sulfate Chemical compound CCCCCCCCCCCCOS(O)(=O)=O MOTZDAYCYVMXPC-UHFFFAOYSA-N 0.000 claims description 5
- 239000000126 substance Substances 0.000 claims description 5
- TWRXJAOTZQYOKJ-UHFFFAOYSA-L Magnesium chloride Chemical compound [Mg+2].[Cl-].[Cl-] TWRXJAOTZQYOKJ-UHFFFAOYSA-L 0.000 claims description 4
- 229940043264 dodecyl sulfate Drugs 0.000 claims description 4
- 239000000084 colloidal system Substances 0.000 claims description 3
- 239000008367 deionised water Substances 0.000 claims description 2
- 229910021641 deionized water Inorganic materials 0.000 claims description 2
- 238000007598 dipping method Methods 0.000 claims description 2
- 235000015110 jellies Nutrition 0.000 claims description 2
- 239000008274 jelly Substances 0.000 claims description 2
- 229910001629 magnesium chloride Inorganic materials 0.000 claims description 2
- 238000000643 oven drying Methods 0.000 claims 1
- 229910044991 metal oxide Inorganic materials 0.000 abstract description 11
- 150000004706 metal oxides Chemical class 0.000 abstract description 11
- 239000002131 composite material Substances 0.000 abstract description 8
- RJZNFXWQRHAVBP-UHFFFAOYSA-I aluminum;magnesium;pentahydroxide Chemical compound [OH-].[OH-].[OH-].[OH-].[OH-].[Mg+2].[Al+3] RJZNFXWQRHAVBP-UHFFFAOYSA-I 0.000 abstract description 4
- 230000003446 memory effect Effects 0.000 abstract description 3
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- 238000000975 co-precipitation Methods 0.000 description 7
- 239000012153 distilled water Substances 0.000 description 7
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- 239000011734 sodium Substances 0.000 description 6
- 239000004743 Polypropylene Substances 0.000 description 5
- 229920001155 polypropylene Polymers 0.000 description 5
- 239000002202 Polyethylene glycol Substances 0.000 description 4
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 4
- 229910052760 oxygen Inorganic materials 0.000 description 4
- 239000001301 oxygen Substances 0.000 description 4
- 229920001223 polyethylene glycol Polymers 0.000 description 4
- 229920000642 polymer Polymers 0.000 description 4
- 229920002292 Nylon 6 Polymers 0.000 description 3
- 230000009286 beneficial effect Effects 0.000 description 3
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- 238000012986 modification Methods 0.000 description 3
- 238000000634 powder X-ray diffraction Methods 0.000 description 3
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 2
- 239000004372 Polyvinyl alcohol Substances 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 2
- GSWGDDYIUCWADU-UHFFFAOYSA-N aluminum magnesium oxygen(2-) Chemical compound [O--].[Mg++].[Al+3] GSWGDDYIUCWADU-UHFFFAOYSA-N 0.000 description 2
- 229910052799 carbon Inorganic materials 0.000 description 2
- 230000002349 favourable effect Effects 0.000 description 2
- 239000007789 gas Substances 0.000 description 2
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 2
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- 239000012528 membrane Substances 0.000 description 2
- ACVYVLVWPXVTIT-UHFFFAOYSA-M phosphinate Chemical compound [O-][PH2]=O ACVYVLVWPXVTIT-UHFFFAOYSA-M 0.000 description 2
- 229910052698 phosphorus Inorganic materials 0.000 description 2
- 239000011574 phosphorus Substances 0.000 description 2
- 229920002451 polyvinyl alcohol Polymers 0.000 description 2
- 239000000779 smoke Substances 0.000 description 2
- 241000894007 species Species 0.000 description 2
- 230000002195 synergetic effect Effects 0.000 description 2
- 230000002194 synthesizing effect Effects 0.000 description 2
- 229910003023 Mg-Al Inorganic materials 0.000 description 1
- 239000004698 Polyethylene Substances 0.000 description 1
- DBMJMQXJHONAFJ-UHFFFAOYSA-M Sodium laurylsulphate Chemical compound [Na+].CCCCCCCCCCCCOS([O-])(=O)=O DBMJMQXJHONAFJ-UHFFFAOYSA-M 0.000 description 1
- 125000000129 anionic group Chemical group 0.000 description 1
- 238000006065 biodegradation reaction Methods 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 229910052599 brucite Inorganic materials 0.000 description 1
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- 239000001913 cellulose Substances 0.000 description 1
- 229920002678 cellulose Polymers 0.000 description 1
- 238000012512 characterization method Methods 0.000 description 1
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- 235000019441 ethanol Nutrition 0.000 description 1
- 238000010304 firing Methods 0.000 description 1
- JEGUKCSWCFPDGT-UHFFFAOYSA-N h2o hydrate Chemical compound O.O JEGUKCSWCFPDGT-UHFFFAOYSA-N 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 238000001027 hydrothermal synthesis Methods 0.000 description 1
- 150000004679 hydroxides Chemical class 0.000 description 1
- 238000011065 in-situ storage Methods 0.000 description 1
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- 238000005342 ion exchange Methods 0.000 description 1
- 229920005610 lignin Polymers 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 239000011777 magnesium Substances 0.000 description 1
- 229910021645 metal ion Inorganic materials 0.000 description 1
- 238000002715 modification method Methods 0.000 description 1
- 239000002114 nanocomposite Substances 0.000 description 1
- 239000002135 nanosheet Substances 0.000 description 1
- 231100000956 nontoxicity Toxicity 0.000 description 1
- 150000002891 organic anions Chemical class 0.000 description 1
- 229920000620 organic polymer Polymers 0.000 description 1
- 239000001814 pectin Substances 0.000 description 1
- 229920001277 pectin Polymers 0.000 description 1
- 235000010987 pectin Nutrition 0.000 description 1
- 230000035699 permeability Effects 0.000 description 1
- 229920000747 poly(lactic acid) Polymers 0.000 description 1
- 229920000573 polyethylene Polymers 0.000 description 1
- 239000004626 polylactic acid Substances 0.000 description 1
- 239000002861 polymer material Substances 0.000 description 1
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- 229920002554 vinyl polymer Polymers 0.000 description 1
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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
- D06M11/73—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 with carbon or compounds thereof
- D06M11/76—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 with carbon or compounds thereof with carbon oxides or carbonates
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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
- D06M11/32—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 with oxygen, ozone, ozonides, oxides, hydroxides or percompounds; Salts derived from anions with an amphoteric element-oxygen bond
- D06M11/36—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 with oxygen, ozone, ozonides, oxides, hydroxides or percompounds; Salts derived from anions with an amphoteric element-oxygen bond with oxides, hydroxides or mixed oxides; with salts derived from anions with an amphoteric element-oxygen bond
- D06M11/44—Oxides or hydroxides of elements of Groups 2 or 12 of the Periodic Table; Zincates; Cadmates
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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
- D06M11/32—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 with oxygen, ozone, ozonides, oxides, hydroxides or percompounds; Salts derived from anions with an amphoteric element-oxygen bond
- D06M11/36—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 with oxygen, ozone, ozonides, oxides, hydroxides or percompounds; Salts derived from anions with an amphoteric element-oxygen bond with oxides, hydroxides or mixed oxides; with salts derived from anions with an amphoteric element-oxygen bond
- D06M11/45—Oxides or hydroxides of elements of Groups 3 or 13 of the Periodic Table; Aluminates
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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
- D06M11/51—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 with sulfur, selenium, tellurium, polonium or compounds thereof
- D06M11/55—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 with sulfur, selenium, tellurium, polonium or compounds thereof with sulfur trioxide; with sulfuric acid or thiosulfuric acid or their salts
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- 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
- D06M11/68—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 with phosphorus or compounds thereof, e.g. with chlorophosphonic acid or salts thereof
- D06M11/70—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 with phosphorus or compounds thereof, e.g. with chlorophosphonic acid or salts thereof with oxides of phosphorus; with hypophosphorous, phosphorous or phosphoric acids or their salts
- D06M11/71—Salts of phosphoric acids
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- 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
- D06M13/244—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 sulfur or phosphorus
- D06M13/248—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 sulfur or phosphorus with compounds containing sulfur
- D06M13/262—Sulfated compounds thiosulfates
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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
- D06M2101/04—Vegetal fibres
- D06M2101/06—Vegetal fibres cellulosic
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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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- Engineering & Computer Science (AREA)
- Textile Engineering (AREA)
- Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)
- Chemical Or Physical Treatment Of Fibers (AREA)
Abstract
The invention belongs to the technical field of textile after-finishing, and particularly relates to a preparation method and application of magnesium-aluminum hydrotalcite flame-retardant modified jute fabric with different anion intercalation layers. The method comprises the following steps: preparation of Cl by coprecipitation‑And (2) intercalated layered magnesium aluminum hydroxide (LDH), roasting the intercalated layered magnesium aluminum hydroxide (LDH) to form layered double metal oxide (LDO), simultaneously washing the jute fabric, soaking the jute fabric in solution containing different anions, then adding the LDO into the anion solution, stirring for reaction by utilizing the structure memory effect, separating and drying to obtain the magnesium aluminum hydrotalcite loaded modified jute fabric with different anions. The preparation method is simple and convenient, and the obtained composite sample has good interface binding property and excellent flame retardant property.
Description
Technical Field
The invention belongs to the technical field of textile after-finishing, and particularly relates to a preparation method and application of magnesium-aluminum hydrotalcite flame-retardant modified jute fabric with different anion intercalation layers.
Background
Layered double hydroxides (LDHs for short) are anionic layered materials which can be artificially synthesized according to specific functional requirements. Its structure is similar to brucite, generally composed of MO6The octahedrons are coterminous with each other to form a main body laminate, and anions are mainly distributed among the layers to balance the overall charge. The metal ions are uniformly distributed on the laminate in a certain mode, and the main laminate and the interlayer are associated through hydrogen bonds, electrostatic interaction or coordination bonds. LDHs have the following properties: (1) the anions between the layers can be exchanged; (2) the composition and structure can also be regulated and controlled generally; (3) the thermal stability is better; (4) structural memory effect. The structure memory effect means that the LDHs can be destroyed into composite metal oxide after being roasted at a certain temperature; however, after the calcined substance is put into water or a solution containing anions, the calcined substance can be changed back to the original layered structure, and the anions in the solution are introduced between layers. The special structural property and thermal property determine that the flame retardant can be used as a flame retardant in a high polymer material. Considerable amount of water molecules are adsorbed between molecular layers of the LDHs, and a large number of hydroxyl groups are arranged on the surface of the LDHs. Under high temperature, hydrotalcite filled in polymer can lose interlayer water and hydroxyl on laminate to dehydrate and emit in the form of water vapor, and water and CO released by decomposition2The gas absorbs a large amount of heat and dilutes the concentration of oxygen to lower the temperature of the polymer combustion surface, preventing further degradation of the polymer, and acting as a flame retardant. In addition, the special laminated structure endows the flame-retardant flame.
LDHs have been reported as flame retardants effective in improving the flame retardant properties of organic polymers, such as LDH composite polypropylene (PP) (see Gao Y, Zhang Y, Williams G R, et al. Layered double hydroxide-oxidized carbon n-nonwoven fibers as high effective flame retardant fibers [ J ]. Scientific reports, 2016, 6: 502.), polyvinyl alcohol (PVA) (see Dinari M, Nabiyan A. Citrio acid-modified laminated fibers as a green reinforcing fibers for improving Thermal properties and mechanical properties of poly (vinyl) -base ] J.M.J.. polyethylene glycol, polyethylene glycol, polyethylene glycol, polyethylene glycol, polyethylene, 2016, 34(5): 542 & lt- & gt 551.), nylon 6 (PA 6) (see L.C. Du, B.J. Qu, M.Zhang, Thermal properties and comfort characteristics of nylon 6/MgAl-LDH nanocomposites vision improvement and molecular characterization. Degrad. Stab 2007, 92(3), 497 & lt- & gt 502.), polylactic acid (see Lu S, Hong W, Chen. Nanorenformation of Two-Dimensional Nanomatics for film Polymeric compositions: An Overview [ J ]. Advances in polymers Technology, 2019, 2019), etc., show good application prospects.
Patent (application number) 201811612038.9 discloses a dialkyl hypophosphite intercalated hydrotalcite-enhanced flame-retardant polypropylene composite material, which adopts an ion exchange method to synthesize dialkyl hypophosphite intercalated hydrotalcite, improves the compatibility between hydrotalcite and polypropylene by modifying hydrotalcite with organic anion dialkyl hypophosphite ions, and utilizes the synergistic flame-retardant function of the dialkyl hypophosphite ions and the hydrotalcite to ensure that the modified polypropylene composite material obtains good flame-retardant performance.
Patent (application number) 201811355853.1 discloses a flame-retardant wallpaper filled with bismuth oxyhydroxide, which is prepared by in-situ synthesizing bismuth oxyhydroxide by hydrothermal reaction, inserting the bismuth oxyhydroxide between sheets of Mg-Al hydrotalcite nanosheets, adding papermaking slurry, and preparing the flame-retardant wallpaper by subsequent processes, wherein most of the oxygen indexes of the obtained samples are higher than 27, and most of the flame-retardant grades reach V-1 grade.
Currently, there are few reports and concerns about the study of compounding LDHs with natural fibers to improve flame retardant properties. The jute fiber has the excellent characteristics of moisture absorption and wet permeability, good dyeing property, low price, environmental protection, easy biodegradation and the like, and has high strength, low extension, good heat insulation and sound absorption effects, so that the jute fiber obtains wide application space in the aspects of automotive interiors such as linings, seat inner plates, sound box plates and the like. However, the jute fibers and the composite materials thereof have generally low limiting oxygen index and belong to inflammable substances or combustible substances, and a proper flame retardant is added for modification so as to effectively reduce the potential safety hazard. At present, organic phosphorus flame retardants are commonly used in the market for modifying the flame retardants, but the flame retardants are mostly liquid at room temperature, are easy to drip at high temperature, have large smoke quantity and toxicity, and are limited to a certain extent in application. Considering that LDHs have the excellent characteristics of no toxicity, no dripping, high decomposition temperature, good stability, smoke suppression, simple and convenient synthesis and the like, the flame-retardant modified jute fiber has good performance expectation, and the jute fiber contains high-hydroscopicity components such as cellulose, lignin, pectin and the like, is very suitable for being combined with LDHs with strong polarity and is beneficial to forming good interface binding property of the LDHs and the LDHs.
Disclosure of Invention
In order to realize better adhesion and flame-retardant modification of LDH to jute fiber, the invention provides a post-finishing method for reconstructing magnesium-aluminum hydrotalcite modified jute fabric with various anions in an insertion layer by roasting, and particularly discloses a preparation method and application of magnesium-aluminum hydrotalcite flame-retardant modified jute fabric with different anion insertions, wherein the preparation method comprises the following steps: preparation of Cl by coprecipitation-And (2) intercalated layered magnesium aluminum hydroxide (LDH), roasting the intercalated layered magnesium aluminum hydroxide (LDH) to form layered double metal oxide (LDO), simultaneously washing the jute fabric, soaking the jute fabric in a solution containing different anion types, then adding the LDO into the anion solution, stirring for reaction, separating and drying to obtain the different anion intercalated magnesium aluminum hydrotalcite-loaded modified jute fabric.
The technical scheme of the invention is realized as follows:
the preparation method of the flame-retardant modified jute fabric with the magnalium hydrotalcite intercalated with different anions comprises the following steps:
(1) separately preparing a solution containing MgCl2、AlCl3Slowly dripping the NaOH solution into the mixed solution, and adjusting the pH value to 9.5 to obtain magnalium hydrotalcite jelly;
(2) standing and aging the magnalium hydrotalcite colloid prepared in the step (1) for 2 hours, filtering, placing the filtrate in an oven for drying to obtain magnalium hydrotalcite blocky solid, grinding into powder, placing the magnalium hydrotalcite into a muffle furnace, heating and calcining in air atmosphere, and naturally cooling to room temperature to obtain layered bimetallic oxide;
(3) sequentially soaking and washing jute cloth samples by deionized water and ethanol, and drying in an oven to obtain a pretreated jute fabric;
(4) and (3) dipping the pretreated jute fabric into a solution containing anions, completely soaking for 0.08-0.5h, then adding the layered bimetal oxide obtained in the step (2), stirring for 0.5-3h, taking out the fabric, and placing the fabric in an oven for drying to obtain the magnalium hydrotalcite flame-retardant modified jute fabric with different anion intercalation.
Mg in the mixed solution in the step (1)2+And Al3+The molar ratio was 3:1, the total ion concentration was 0.5mol/L, and the mass concentration of the NaOH solution was 6 mol/L.
The drying temperature in the oven in the step (2) is 100-110 ℃.
In the step (2), the heating rate of the heating calcination is 5 ℃/min, the calcination temperature is 500 ℃, and the calcination time is 1-3 h.
The temperature for drying in the oven in the step (3) is 80 ℃.
The anion in the step (4) is CO3 2-、SO4 2-、HPO4 2-Or dodecyl sulfate radical ion, anion concentration of 0.02-0.9 mol/L, and solution temperature of 25 deg.C.
The mass ratio of the jute fabric to the layered double oxide in the step (4) is 1 (0.07-2.14), and the mass concentration of the layered double oxide is 0.33-10 g/L.
The drying temperature of the oven in the step (4) is 60-100 ℃, and the drying time is 6-12 h.
The prepared magnalium hydrotalcite flame-retardant modified jute fabric.
The application of the magnalium hydrotalcite flame-retardant modified jute fabric in the preparation of flame-retardant materials.
The invention has the following beneficial effects:
1. the method for synthesizing the new green nano flame retardant LDH by roasting reconstruction is favorable for directly loading the new green nano flame retardant LDH on the jute fabric, so that the green nano flame retardant LDH and the jute fabric can obtain better interface bonding performance and is favorable for loading the LDH;
2. according to the invention, various anions of different types and different ion sizes can be intercalated into LDH layers by a roasting reconstruction method, so that the LDH modified jute fabric beneficial to improving the flame retardant effect is obtained. The experimental results show that CO3 2-When the adhesion amount of the intercalated LDH is 17.5 percent of the mass of the jute fabric, the flame retardant effect of the intercalated LDH on the jute fabric can be improved by 86.6 percent. At the same time, compare with CO3 2-、SO4 2-Magnesium-aluminum LDH modified jute fabrics, HPO, intercalated with dodecyl sulfate ions (DS)4 2-The flame retardant property of the intercalated magnesium-aluminum LDH modified jute fabric is optimal.
3. The preparation method is simple and convenient, and the obtained composite sample has good interface binding property and excellent flame retardant property. The flame-retardant modification method provides a basis for developing the lower-cost multifunctional jute fiber with excellent flame-retardant property, and the jute fiber can play a greater role in the fields of home textiles, automotive interiors and the like.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, it is obvious that the drawings in the following description are only some embodiments of the present invention, and for those skilled in the art, other drawings can be obtained according to the drawings without creative efforts.
FIG. 1 is Cl prepared in example 1-X-ray powder of intercalated magnesium-aluminum LDHDiffraction pattern.
Fig. 2 is an X-ray powder diffraction pattern of layered magnesium aluminum oxide (LDO) prepared in example 1.
FIG. 3 shows CO prepared in example 13 2-And (3) an electron scanning microscope picture of the surface of the jute fabric modified by the intercalated magnesium-aluminum LDH.
FIG. 4 shows the horizontal burning rate, CO, of the modified jute fabric prepared in example 13 2-And (3) a curve graph of the relation between the loading amount of the intercalated magnesium-aluminum LDH and the addition amount of the LDO.
Fig. 5 is a bar graph of sample horizontal burn rate versus intercalated anion species for different anion intercalated magnesium aluminum LDH modified jute fabrics prepared according to examples 1, 5, 6, 7 at the same jute fabric to LDH loading mass ratio.
Detailed Description
The technical solutions of the present invention will be described clearly and completely below with reference to embodiments of the present invention, and it should be apparent that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be obtained by a person skilled in the art based on the embodiments of the present invention without inventive step, are within the scope of the present invention.
Example 1
One embodiment of the present example reforms CO by calcination3 2-The method for modifying the jute fabric by intercalated magnesium-aluminum LDH flame retardation specifically comprises the following steps:
(1) preparation of Cl by coprecipitation method-Intercalation magnalium LDH: according to Mg2+：Al3+The molar ratio is 3:1, the total ion concentration is 0.5mol/L, 700mL of MgCl is prepared2、AlCl3200mL of 6mol/L NaOH solution was prepared. The NaOH solution was slowly added dropwise to the mixed solution until the pH became 9.5, finally obtaining LDH gum. Standing and aging for 2 hours, filtering the solution, putting the filtrate into a 110 ℃ oven, and completely drying to obtain the LDH blocky solid. Grinding into powder for use.
(2) Preparation of layered double metal oxide (LDO) by a roasting process: and putting the LDH which is ground into powder into a muffle furnace, calcining for 2 hours at 500 ℃ in the air atmosphere at the heating rate of 5 ℃/min, and naturally cooling to room temperature to obtain the LDO.
(3) LDO load jute cloth:
pretreatment of jute fabric: taking jute fabric with length and width of 6cm × 6cm (gram weight 390 g/m)2) Soaking the seeds in distilled water for 5 min, and soaking the seeds in absolute ethyl alcohol for 5 min. Drying at 80 ℃ for later use.
② preparing Na with the volume of 300mL and the concentration of 0.1mol/L2CO3The solution was maintained at a temperature of 25 ℃. And (3) placing the pretreated jute fabric in the solution, adding 0.5g of LDO after the jute fabric is completely soaked in the solution for 5 minutes, stirring and reacting for 2 hours, directly taking out the jute fabric, and drying the jute fabric in an oven at the temperature of 80 ℃ for 8 hours. Weighing to obtain CO3 2-The intercalated LDH-loaded modified jute fabric samples.
FIG. 1 is Cl prepared according to this example-X-ray powder diffraction pattern of intercalated magnesium aluminum LDH. The characteristic peaks at 11.3 degrees and 22.7 degrees show the typical layered structure of the hydrotalcite material, which respectively correspond to the (003) and (006) crystal planes of the material. The corresponding diffraction peaks have certain peak broadening, which indicates that the synthesized Cl-The intercalation magnalium LDH has at least one dimension of nanometer size. In addition, the sharp peak type shows that the crystallinity of the magnesium-aluminum LDH is better.
Fig. 2 is an X-ray powder diffraction pattern of the LDO prepared according to this example. The characteristic peaks of the LDH at 6.6 degrees, 16.7 degrees, 20.5 degrees and 23.3 correspond to aluminum magnesium oxide compounds, which shows that the LDH loses interlayer anions after calcination, and the obtained LDO has no obvious layered structure any more. The larger half-peak width and certain diffraction peak intensity of the diffraction peak indicate that the LDO size is still in the nanometer level, but the crystallinity is slightly poor.
FIG. 3 is CO prepared according to this example3 2-And (3) an electron scanning microscope picture of the surface of the jute fabric modified by the intercalated magnesium-aluminum LDH. As can be seen from FIG. (a), the CO formed is reconstituted by calcination3 2-The intercalated magnesium-aluminum LDH is uniformly attached to jute fibers in the form of bubbles;from the graph (b), CO can be seen more closely3 2-The intercalation magnesium aluminum LDH is uniformly coated on the surface of jute fiber in the form of a membrane, and along the texture structure of the fiber, part of LDH is convex and bubbly at the position of the break-off adhesion, which is caused by gas phase escaping in the process of drying an LDH colloid membrane formed by roasting reconstruction in an oven.
Example 2
One embodiment of the present example reforms CO by calcination3 2-The method for modifying the jute fabric by intercalated magnesium-aluminum LDH flame retardation specifically comprises the following steps:
(1) preparation of Cl by coprecipitation method-Intercalation magnalium LDH: according to Mg2+：Al3+The molar ratio is 3:1, the total ion concentration is 0.5mol/L, 700mL of MgCl is prepared2、AlCl3200mL of 6mol/L NaOH solution was prepared. The NaOH solution was slowly added dropwise to the mixed solution until the pH became 9.5, finally obtaining LDH gum. Standing and aging for 2 hours, filtering the solution, putting the filtrate into a 110 ℃ oven, and completely drying to obtain the LDH blocky solid. Grinding into powder for use.
(2) Preparation of layered double metal oxide (LDO) by a roasting process: and putting the LDH which is ground into powder into a muffle furnace, calcining for 2 hours at 500 ℃ in the air atmosphere at the heating rate of 5 ℃/min, and naturally cooling to room temperature to obtain the LDO.
(3) LDO load jute cloth:
pretreatment of jute fabric: taking a jute fabric with the length and width of 6cm multiplied by 6cm (the gram weight is 390 g/m)2) Soaking the seeds in distilled water for 5 min, and soaking the seeds in absolute ethyl alcohol for 5 min. Drying at 80 ℃ for later use.
② preparing Na with the volume of 300mL and the concentration of 0.1mol/L2CO3The solution was maintained at a temperature of 25 ℃. And (3) placing the pretreated jute fabric in the solution, adding 3g of LDO after the jute fabric is completely soaked in the solution for 5 minutes, stirring and reacting for 2 hours, directly taking out the jute fabric, and drying the jute fabric in an oven at the temperature of 80 ℃ for 8 hours. Weighing to obtain CO3 2-The intercalated LDH-loaded modified jute fabric samples.
Example 3
One embodiment of the present example reforms CO by calcination3 2-The method for modifying the jute fabric by intercalated magnesium-aluminum LDH flame retardation specifically comprises the following steps:
(1) preparation of Cl by coprecipitation method-Intercalation magnalium LDH: according to Mg2+：Al3+The molar ratio is 3:1, the total ion concentration is 0.5mol/L, 700mL of MgCl is prepared2、AlCl3200mL of 6mol/L NaOH solution was prepared. The NaOH solution was slowly added dropwise to the mixed solution until the pH became 9.5, finally obtaining LDH gum. Standing and aging for 2 hours, filtering the solution, putting the filtrate into a 110 ℃ oven, and completely drying to obtain the LDH blocky solid. Grinding into powder for use.
(2) Preparation of layered double metal oxide (LDO) by a roasting process: and putting the LDH which is ground into powder into a muffle furnace, calcining for 2 hours at 500 ℃ in the air atmosphere at the heating rate of 5 ℃/min, and naturally cooling to room temperature to obtain the LDO.
(3) LDO load jute cloth:
pretreatment of jute fabric: taking jute fabric with length and width of 6cm × 6cm (gram weight 390 g/m)2) Soaking the seeds in distilled water for 5 min, and soaking the seeds in absolute ethyl alcohol for 5 min. Drying at 80 ℃ for later use.
② preparing Na with the volume of 300mL and the concentration of 0.02mol/L2CO3The solution was maintained at a temperature of 25 ℃. And (3) placing the pretreated jute fabric in the solution, adding 0.5g of LDO after the jute fabric is completely soaked in the solution for 5 minutes, stirring and reacting for 2 hours, directly taking out the jute fabric, and drying the jute fabric in an oven at 80 ℃ for 8 hours. Weighing to obtain CO3 2-The intercalated LDH-loaded modified jute fabric samples.
Example 4
One embodiment of the present example reforms CO by calcination3 2-The method for modifying the jute fabric by intercalated magnesium aluminum LDH flame retardation specifically comprises the following steps:
(1) preparation of Cl by coprecipitation method-Intercalation magnalium LDH: according to Mg2+：Al3+The molar ratio is 3:1, the total ion concentration is 0.5mol/L, 700mL of MgCl is prepared2、AlCl3200mL of 6mol/L NaOH solution was prepared. The NaOH solution was slowly added dropwise to the mixed solution until the pH became 9.5, finally obtaining LDH gum. Standing and aging for 2 hours, filtering the solution, putting the filtrate into a 110 ℃ oven, and completely drying to obtain the LDH blocky solid. Grinding into powder for use.
(2) Preparation of layered double metal oxide (LDO) by firing method: and putting the LDH which is ground into powder into a muffle furnace, calcining for 2 hours at 500 ℃ in the air atmosphere at the heating rate of 5 ℃/min, and naturally cooling to room temperature to obtain the LDO.
(3) LDO load jute cloth:
pretreatment of jute fabric: taking jute fabric with length and width of 6cm × 6cm (gram weight 390 g/m)2) Soaking the seeds in distilled water for 5 min, and soaking the seeds in absolute ethyl alcohol for 5 min. Drying at 80 ℃ for later use.
② preparing Na with the volume of 300mL and the concentration of 0.9mol/L2CO3The solution was maintained at a temperature of 25 ℃. And (3) placing the pretreated jute fabric in the solution, adding 0.5g of LDO after the jute fabric is completely soaked in the solution for 5 minutes, stirring and reacting for 2 hours, directly taking out the jute fabric, and drying the jute fabric in an oven at 80 ℃ for 8 hours. Weighing to obtain CO3 2-The intercalated LDH-loaded modified jute fabric samples.
Example 5
Reconstruction of SO by calcination of one of the examples4 2-The method for modifying the jute fabric by intercalated magnesium aluminum LDH flame retardation specifically comprises the following steps:
(1) preparation of Cl by coprecipitation method-Intercalation magnalium LDH: according to Mg2+：Al3+The molar ratio is 3:1, the total ion concentration is 0.5mol/L, 700mL MgCl is prepared2、AlCl3200mL of 6mol/L NaOH solution was prepared. The NaOH solution was slowly added dropwise to the mixed solution until the pH became 9.5, finally obtaining LDH gum. Standing and aging for 2 hours, filtering the solution, putting the filtrate into a 110 ℃ oven, and completely drying to obtain LDH blocksAs a solid. Grinding into powder for use.
(2) Preparation of layered double metal oxide (LDO) by a roasting process: and putting the LDH which is ground into powder into a muffle furnace, calcining for 2 hours at 500 ℃ in the air atmosphere at the heating rate of 5 ℃/min, and naturally cooling to room temperature to obtain the LDO.
(3) LDO load jute cloth:
pretreatment of jute fabric: taking a jute fabric with the length and width of 6cm multiplied by 6cm (the gram weight is 390 g/m)2) Soaking the seeds in distilled water for 5 min, and soaking the seeds in absolute ethyl alcohol for 5 min. Drying at 80 ℃ for later use.
② preparing Na with the volume of 300mL and the concentration of 0.1mol/L2SO4The solution was maintained at a temperature of 25 ℃. And (3) placing the pretreated jute fabric in the solution, adding 0.5g of LDO after the jute fabric is completely soaked in the solution for 5 minutes, stirring and reacting for 2 hours, directly taking out the jute fabric, and drying the jute fabric in an oven at 80 ℃ for 8 hours. Weighing to obtain SO4 2-The intercalated LDH-loaded modified jute fabric samples.
Example 6
Reconstitution of HPO by calcination of one of the examples4 2-The method for modifying the jute fabric by intercalated magnesium-aluminum LDH flame retardation specifically comprises the following steps:
(1) preparation of Cl by coprecipitation method-Intercalation magnalium LDH: according to Mg2+：Al3+The molar ratio is 3:1, the total ion concentration is 0.5mol/L, 700mL of MgCl is prepared2、AlCl3200mL of 6mol/L NaOH solution was prepared. The NaOH solution was slowly added dropwise to the mixed solution until the pH became 9.5, finally obtaining LDH gum. Standing and aging for 2 hours, filtering the solution, putting the filtrate into a 110 ℃ oven, and completely drying to obtain the LDH blocky solid. Grinding into powder for use.
(2) Preparation of layered double metal oxide (LDO) by a roasting process: and putting the LDH which is ground into powder into a muffle furnace, calcining for 2 hours at 500 ℃ in the air atmosphere at the heating rate of 5 ℃/min, and naturally cooling to room temperature to obtain the LDO.
(3) LDO load jute cloth:
pretreatment of jute fabric: taking a jute fabric with the length and width of 6cm multiplied by 6cm (the gram weight is 390 g/m)2) Soaking the seeds in distilled water for 5 min, and soaking the seeds in absolute ethyl alcohol for 5 min. Drying at 80 ℃ for later use.
② preparing Na with the volume of 300mL and the concentration of 0.1mol/L2HPO4The solution was maintained at a temperature of 25 ℃. And (3) placing the pretreated jute fabric in the solution, adding 0.5g of LDO after the jute fabric is completely soaked in the solution for 5 minutes, stirring and reacting for 2 hours, directly taking out the jute fabric, and drying the jute fabric in an oven at 80 ℃ for 8 hours. Weighing to obtain HPO4 2-The intercalated LDH-loaded modified jute fabric samples.
Example 7
The method for reconstructing the flame-retardant modified jute fabric by calcining dodecyl sulfuric acid and ion (DS) intercalated magnesium-aluminum LDH comprises the following steps:
(1) preparation of Cl by coprecipitation method-Intercalation magnalium LDH: according to Mg2+：Al3+The molar ratio is 3:1, the total ion concentration is 0.5mol/L, 700mL MgCl is prepared2、AlCl3200mL of 6mol/L NaOH solution was prepared. The NaOH solution was slowly added dropwise to the mixed solution until the pH became 9.5, finally obtaining LDH gum. Standing and aging for 2 hours, filtering the solution, putting the filtrate into a 110 ℃ oven, and completely drying to obtain LDH blocky solid. Grinding into powder for use.
(2) Preparation of layered double metal oxide (LDO) by a roasting process: and putting the LDH which is ground into powder into a muffle furnace, calcining for 2 hours at 500 ℃ in the air atmosphere at the heating rate of 5 ℃/min, and naturally cooling to room temperature to obtain the LDO.
(3) LDO load jute cloth:
pretreatment of jute fabric: taking a jute fabric with the length and width of 6cm multiplied by 6cm (the gram weight is 390 g/m)2) Soaking the seeds in distilled water for 5 min, and soaking the seeds in absolute ethyl alcohol for 5 min. Drying at 80 ℃ for later use.
② preparing a dodecyl sodium sulfate solution with the volume of 300mL and the concentration of 0.1mol/L, and keeping the temperature of the solution at 25 ℃. And (3) placing the pretreated jute fabric in the solution, adding 0.5g of LDO after the jute fabric is completely soaked in the solution for 5 minutes, stirring and reacting for 2 hours, directly taking out the jute fabric, and drying the jute fabric in an oven at the temperature of 80 ℃ for 8 hours. And weighing to obtain a sample of the DS-LDH load modified jute fabric.
Examples of the effects of the invention
CO prepared in example 13 2-Intercalation magnalium LDH modified jute fabric and horizontal burning characteristic and CO thereof3 2-The relationship between the loading amount of the intercalated magnesium aluminum LDH on the jute fabric and the LDO adding amount is shown in figure 4. As can be seen, as the addition of LDO is increased, CO on jute fabric3 2-The loading capacity of the intercalated magnesium-aluminum LDH shows a trend that the loading capacity is increased firstly and then reduced and then increased, and the horizontal burning rate of the modified jute fabric shows a continuous reduction trend, which indicates that the CO is3 2-The intercalated magnesium-aluminum LDH has obvious flame retardant effect on jute fabrics. When the LDO adding amount is 0.9g, CO3 2-The loading capacity of the intercalated magnesium aluminum LDH can reach 0.245g, and the weight ratio of the intercalated magnesium aluminum LDH to jute fabric is 17.5%. At the moment, the flame retardant effect on jute fabrics can be improved by 86.6 percent; when the LDO adding amount is 0.5g, CO3 2-The loading capacity of the intercalated magnesium-aluminum LDH can reach 0.227g, and the flame retardant effect on jute fabrics can be improved by 53.8 percent; considering the cost performance of the materials, the optimal dosage of the LDO can be determined to be 0.5 g.
The different anion intercalation magnalium LDH modified jute fabrics prepared by examples 1, 5, 6 and 7 have the relationship between the horizontal burning rate of the sample and the species of intercalation anions under the same jute fabric and LDH loading mass ratio as shown in figure 5. Compared with CO3 2-、SO4 2-Magnesium-aluminum LDH modified jute fabrics, HPO, intercalated with dodecyl sulfate ions (DS)4 2-The horizontal burning rate (0.029 cm/s) of the jute fabric modified by the intercalated magnesium-aluminum LDH is the lowest, namely the jute fabric has the best flame retardant property. Compared with CO, the flame retardant effect of the composition on jute fabric3 2-The intercalation magnalium LDH can be increased by 1.96 times. Thus illustrating HPO4 2-After intercalation enters into magnesium-aluminum LDH interlamination, phosphorus system can be volatilizedThe flame retardant has the flame retardant effect (namely, absorbs heat during decomposition, and can enable a formed carbon layer to be more compact and uniform), so that the flame retardant has a synergistic flame retardant function with the LDH with a reconstructed structure (the LDH also decomposes and absorbs a large amount of heat, and forms a composite metal oxide layer to cover the surface of a material, so that the oxygen entry and heat radiation are blocked, the heat release rate is rapidly reduced), and a better flame retardant effect is generated.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and should not be taken as limiting the scope of the present invention, which is intended to cover any modifications, equivalents, improvements, etc. within the spirit and scope of the present invention.
Claims (8)
1. The preparation method of the flame-retardant modified jute fabric with the magnalium hydrotalcite intercalated with different anions is characterized by comprising the following steps:
(1) separately preparing a solution containing MgCl2、AlCl3Slowly dripping the NaOH solution into the mixed solution, and adjusting the pH value to 9.5 to obtain magnalium hydrotalcite jelly; mg in the mixed solution2+And Al3+The molar ratio is 3:1, the total ion concentration is 0.5mol/L, and the substance concentration of the NaOH solution is 6 mol/L;
(2) standing and aging the magnalium hydrotalcite colloid prepared in the step (1) for 2 hours, filtering, placing the filtrate in an oven for drying to obtain magnalium hydrotalcite blocky solid, grinding into powder, placing the magnalium hydrotalcite into a muffle furnace, heating and calcining in air atmosphere, and naturally cooling to room temperature to obtain layered bimetallic oxide; wherein the heating rate of the heating calcination is 5 ℃/min, the calcination temperature is 500 ℃, and the calcination time is 1-3 h;
(3) sequentially soaking and washing jute cloth samples by deionized water and ethanol, and drying in an oven to obtain a pretreated jute fabric;
(4) and (3) dipping the pretreated jute fabric into a solution containing anions, completely soaking for 0.08-0.5h, then adding the layered bimetal oxide obtained in the step (2), stirring for 0.5-3h, taking out the fabric, and placing the fabric in an oven for drying to obtain the magnalium hydrotalcite flame-retardant modified jute fabric with different anion intercalation.
2. The method for preparing the flame-retardant modified jute fabric with magnesium-aluminum hydrotalcite intercalated by different anions according to claim 1, wherein the method comprises the following steps: the temperature of the oven drying in the step (2) is 100-110 ℃.
3. The method for preparing the magnesium aluminum hydrotalcite flame retardant modified jute fabric with different anion intercalation according to claim 1, wherein the method comprises the following steps: the temperature for drying in the oven in the step (3) is 80 ℃.
4. The method for preparing the flame-retardant modified jute fabric with magnesium-aluminum hydrotalcite intercalated by different anions according to claim 1, wherein the method comprises the following steps: the anion in the step (4) is CO3 2-、SO4 2-、HPO4 2-Or dodecyl sulfate radical ion, anion concentration of 0.02-0.9 mol/L, and solution temperature of 25 deg.C.
5. The method for preparing the flame-retardant modified jute fabric with magnesium-aluminum hydrotalcite intercalated by different anions according to claim 1, wherein the method comprises the following steps: the mass ratio of the jute fabric to the layered double oxide in the step (4) is 1 (0.07-2.14), and the mass concentration of the layered double oxide is 0.33-10 g/L.
6. The method for preparing the flame-retardant modified jute fabric with magnesium-aluminum hydrotalcite intercalated by different anions according to claim 1, wherein the method comprises the following steps: the drying temperature of the oven in the step (4) is 60-100 ℃, and the drying time is 6-12 h.
7. The flame retardant modified jute fabric made from the magnesium aluminum hydrotalcite of any of claims 1 to 6.
8. The use of the magnesium aluminum hydrotalcite flame retardant modified jute fabric of claim 7 in the preparation of flame retardant materials.
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Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2004115964A (en) * | 2002-09-26 | 2004-04-15 | Toagosei Co Ltd | Fabric having refreshing property |
| CN1537807A (en) * | 2003-10-23 | 2004-10-20 | 浙江大学 | Method of preparing bimetal oxide and hydrotalcite |
| JP2006070406A (en) * | 2004-09-06 | 2006-03-16 | Tayca Corp | Fiber material containing lamellar double hydroxide incorporating ascorbic acid |
| CN1837329A (en) * | 2006-03-13 | 2006-09-27 | 浙江大学 | Composite inorganic flame retardant and its preparation method |
| CN101391797A (en) * | 2008-11-06 | 2009-03-25 | 哈尔滨工程大学 | Single anion pillared hydrotalcite and preparation method thereof |
| CN103726303A (en) * | 2013-12-27 | 2014-04-16 | 顶呱呱彩棉服饰有限公司 | Heat-absorption finishing method of colored cotton knitwear |
-
2020
- 2020-01-18 CN CN202010055939.3A patent/CN111074544B/en active Active
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2004115964A (en) * | 2002-09-26 | 2004-04-15 | Toagosei Co Ltd | Fabric having refreshing property |
| CN1537807A (en) * | 2003-10-23 | 2004-10-20 | 浙江大学 | Method of preparing bimetal oxide and hydrotalcite |
| JP2006070406A (en) * | 2004-09-06 | 2006-03-16 | Tayca Corp | Fiber material containing lamellar double hydroxide incorporating ascorbic acid |
| CN1837329A (en) * | 2006-03-13 | 2006-09-27 | 浙江大学 | Composite inorganic flame retardant and its preparation method |
| CN101391797A (en) * | 2008-11-06 | 2009-03-25 | 哈尔滨工程大学 | Single anion pillared hydrotalcite and preparation method thereof |
| CN103726303A (en) * | 2013-12-27 | 2014-04-16 | 顶呱呱彩棉服饰有限公司 | Heat-absorption finishing method of colored cotton knitwear |
Non-Patent Citations (2)
| Title |
|---|
| Nano-Mg–Al-layered double hydroxide application to cotton for enhancing mechanical, UV protection and flame retardancy at low cytotoxicity level;Sunita Barik等;《Cellulose》;20161212(第24期);1107–1120 * |
| Sunita Barik等.Nano-Mg–Al-layered double hydroxide application to cotton for enhancing mechanical, UV protection and flame retardancy at low cytotoxicity level.《Cellulose》.2016,(第24期), * |
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