CN113235183A - Flame-retardant elastic fabric with good moisture absorption and preparation method thereof - Google Patents
Flame-retardant elastic fabric with good moisture absorption and preparation method thereof Download PDFInfo
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- CN113235183A CN113235183A CN202110620816.4A CN202110620816A CN113235183A CN 113235183 A CN113235183 A CN 113235183A CN 202110620816 A CN202110620816 A CN 202110620816A CN 113235183 A CN113235183 A CN 113235183A
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- flame
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- retardant
- elastic fabric
- temperature
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- 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 70
- 239000003063 flame retardant Substances 0.000 title claims abstract description 70
- 239000004744 fabric Substances 0.000 title claims abstract description 57
- 238000010521 absorption reaction Methods 0.000 title claims abstract description 17
- 238000002360 preparation method Methods 0.000 title abstract description 7
- IWDCLRJOBJJRNH-UHFFFAOYSA-N p-cresol Chemical compound CC1=CC=C(O)C=C1 IWDCLRJOBJJRNH-UHFFFAOYSA-N 0.000 claims abstract description 25
- WTDHULULXKLSOZ-UHFFFAOYSA-N Hydroxylamine hydrochloride Chemical compound Cl.ON WTDHULULXKLSOZ-UHFFFAOYSA-N 0.000 claims abstract description 16
- UPMLOUAZCHDJJD-UHFFFAOYSA-N 4,4'-Diphenylmethane Diisocyanate Chemical compound C1=CC(N=C=O)=CC=C1CC1=CC=C(N=C=O)C=C1 UPMLOUAZCHDJJD-UHFFFAOYSA-N 0.000 claims abstract description 13
- 239000004743 Polypropylene Substances 0.000 claims abstract description 13
- 229920003229 poly(methyl methacrylate) Polymers 0.000 claims abstract description 13
- 239000004926 polymethyl methacrylate Substances 0.000 claims abstract description 13
- -1 polypropylene Polymers 0.000 claims abstract description 13
- 229920001155 polypropylene Polymers 0.000 claims abstract description 13
- 239000011347 resin Substances 0.000 claims abstract description 13
- 229920005989 resin Polymers 0.000 claims abstract description 13
- MGNCLNQXLYJVJD-UHFFFAOYSA-N cyanuric chloride Chemical compound ClC1=NC(Cl)=NC(Cl)=N1 MGNCLNQXLYJVJD-UHFFFAOYSA-N 0.000 claims abstract description 9
- 239000002994 raw material Substances 0.000 claims abstract description 7
- GVGUFUZHNYFZLC-UHFFFAOYSA-N dodecyl benzenesulfonate;sodium Chemical compound [Na].CCCCCCCCCCCCOS(=O)(=O)C1=CC=CC=C1 GVGUFUZHNYFZLC-UHFFFAOYSA-N 0.000 claims abstract description 6
- 229940080264 sodium dodecylbenzenesulfonate Drugs 0.000 claims abstract description 6
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 51
- 238000003756 stirring Methods 0.000 claims description 35
- WYURNTSHIVDZCO-UHFFFAOYSA-N Tetrahydrofuran Chemical compound C1CCOC1 WYURNTSHIVDZCO-UHFFFAOYSA-N 0.000 claims description 34
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 claims description 33
- 238000006243 chemical reaction Methods 0.000 claims description 31
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 28
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 21
- YLQBMQCUIZJEEH-UHFFFAOYSA-N tetrahydrofuran Natural products C=1C=COC=1 YLQBMQCUIZJEEH-UHFFFAOYSA-N 0.000 claims description 17
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 16
- 238000010992 reflux Methods 0.000 claims description 15
- 239000000835 fiber Substances 0.000 claims description 14
- 239000012768 molten material Substances 0.000 claims description 14
- FJKROLUGYXJWQN-UHFFFAOYSA-N 4-hydroxybenzoic acid Chemical compound OC(=O)C1=CC=C(O)C=C1 FJKROLUGYXJWQN-UHFFFAOYSA-N 0.000 claims description 12
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 12
- XHXFXVLFKHQFAL-UHFFFAOYSA-N phosphoryl trichloride Chemical compound ClP(Cl)(Cl)=O XHXFXVLFKHQFAL-UHFFFAOYSA-N 0.000 claims description 12
- 239000007818 Grignard reagent Substances 0.000 claims description 10
- 150000004795 grignard reagents Chemical class 0.000 claims description 10
- 238000010438 heat treatment Methods 0.000 claims description 10
- VZGDMQKNWNREIO-UHFFFAOYSA-N tetrachloromethane Chemical compound ClC(Cl)(Cl)Cl VZGDMQKNWNREIO-UHFFFAOYSA-N 0.000 claims description 10
- QIGBRXMKCJKVMJ-UHFFFAOYSA-N Hydroquinone Chemical compound OC1=CC=C(O)C=C1 QIGBRXMKCJKVMJ-UHFFFAOYSA-N 0.000 claims description 8
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims description 7
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 7
- 238000002156 mixing Methods 0.000 claims description 7
- TYJJADVDDVDEDZ-UHFFFAOYSA-M potassium hydrogencarbonate Chemical compound [K+].OC([O-])=O TYJJADVDDVDEDZ-UHFFFAOYSA-M 0.000 claims description 7
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 7
- VTDOZTKLYMTWQU-UHFFFAOYSA-N 2,2-dimethylpropane-1,3-diol phosphoryl trichloride Chemical compound OCC(C)(CO)C.P(=O)(Cl)(Cl)Cl VTDOZTKLYMTWQU-UHFFFAOYSA-N 0.000 claims description 6
- NPDACUSDTOMAMK-UHFFFAOYSA-N 4-Chlorotoluene Chemical compound CC1=CC=C(Cl)C=C1 NPDACUSDTOMAMK-UHFFFAOYSA-N 0.000 claims description 6
- 229940090248 4-hydroxybenzoic acid Drugs 0.000 claims description 6
- VCZNNAKNUVJVGX-UHFFFAOYSA-N 4-methylbenzonitrile Chemical compound CC1=CC=C(C#N)C=C1 VCZNNAKNUVJVGX-UHFFFAOYSA-N 0.000 claims description 6
- ZJHSRWNUEOUFAZ-UHFFFAOYSA-N BrC1C(=O)NC(C1)=O.[N] Chemical compound BrC1C(=O)NC(C1)=O.[N] ZJHSRWNUEOUFAZ-UHFFFAOYSA-N 0.000 claims description 6
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 claims description 6
- 238000001816 cooling Methods 0.000 claims description 6
- 230000007935 neutral effect Effects 0.000 claims description 6
- 238000005406 washing Methods 0.000 claims description 6
- RVWUHFFPEOKYLB-UHFFFAOYSA-N 2,2,6,6-tetramethyl-1-oxidopiperidin-1-ium Chemical compound CC1(C)CCCC(C)(C)[NH+]1[O-] RVWUHFFPEOKYLB-UHFFFAOYSA-N 0.000 claims description 5
- 239000004342 Benzoyl peroxide Substances 0.000 claims description 5
- OMPJBNCRMGITSC-UHFFFAOYSA-N Benzoylperoxide Chemical compound C=1C=CC=CC=1C(=O)OOC(=O)C1=CC=CC=C1 OMPJBNCRMGITSC-UHFFFAOYSA-N 0.000 claims description 5
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 claims description 5
- VSCWAEJMTAWNJL-UHFFFAOYSA-K aluminium trichloride Chemical compound Cl[Al](Cl)Cl VSCWAEJMTAWNJL-UHFFFAOYSA-K 0.000 claims description 5
- 235000019400 benzoyl peroxide Nutrition 0.000 claims description 5
- RDHPKYGYEGBMSE-UHFFFAOYSA-N bromoethane Chemical compound CCBr RDHPKYGYEGBMSE-UHFFFAOYSA-N 0.000 claims description 5
- HWCKGOZZJDHMNC-UHFFFAOYSA-M tetraethylammonium bromide Chemical compound [Br-].CC[N+](CC)(CC)CC HWCKGOZZJDHMNC-UHFFFAOYSA-M 0.000 claims description 5
- 238000009941 weaving Methods 0.000 claims description 5
- 239000012153 distilled water Substances 0.000 claims description 3
- 239000005457 ice water Substances 0.000 claims description 3
- 239000000758 substrate Substances 0.000 claims description 3
- 239000012295 chemical reaction liquid Substances 0.000 claims description 2
- 238000000034 method Methods 0.000 claims description 2
- 230000000694 effects Effects 0.000 abstract description 8
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 abstract description 4
- 239000011574 phosphorus Substances 0.000 abstract description 4
- 229910052698 phosphorus Inorganic materials 0.000 abstract description 4
- 239000000571 coke Substances 0.000 abstract description 3
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 abstract description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 abstract description 2
- 229910052799 carbon Inorganic materials 0.000 abstract description 2
- 229910052801 chlorine Inorganic materials 0.000 abstract description 2
- 125000001309 chloro group Chemical group Cl* 0.000 abstract description 2
- 150000001875 compounds Chemical class 0.000 abstract description 2
- 125000002887 hydroxy group Chemical group [H]O* 0.000 abstract description 2
- 239000012774 insulation material Substances 0.000 abstract description 2
- 229910052760 oxygen Inorganic materials 0.000 abstract description 2
- 239000001301 oxygen Substances 0.000 abstract description 2
- 230000000052 comparative effect Effects 0.000 description 6
- 238000002485 combustion reaction Methods 0.000 description 3
- 238000009987 spinning Methods 0.000 description 2
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N Phenol Chemical compound OC1=CC=CC=C1 ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 description 1
- 238000005903 acid hydrolysis reaction Methods 0.000 description 1
- 238000007792 addition Methods 0.000 description 1
- 230000003796 beauty Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
Classifications
-
- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F8/00—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof
- D01F8/04—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof from synthetic polymers
- D01F8/10—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof from synthetic polymers with at least one other macromolecular compound obtained by reactions only involving carbon-to-carbon unsaturated bonds as constituent
-
- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F1/00—General methods for the manufacture of artificial filaments or the like
- D01F1/02—Addition of substances to the spinning solution or to the melt
- D01F1/07—Addition of substances to the spinning solution or to the melt for making fire- or flame-proof filaments
-
- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F1/00—General methods for the manufacture of artificial filaments or the like
- D01F1/02—Addition of substances to the spinning solution or to the melt
- D01F1/10—Other agents for modifying properties
-
- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F8/00—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof
- D01F8/04—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof from synthetic polymers
- D01F8/06—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof from synthetic polymers with at least one polyolefin as constituent
-
- D—TEXTILES; PAPER
- D03—WEAVING
- D03D—WOVEN FABRICS; METHODS OF WEAVING; LOOMS
- D03D13/00—Woven fabrics characterised by the special disposition of the warp or weft threads, e.g. with curved weft threads, with discontinuous warp threads, with diagonal warp or weft
- D03D13/008—Woven fabrics characterised by the special disposition of the warp or weft threads, e.g. with curved weft threads, with discontinuous warp threads, with diagonal warp or weft characterised by weave density or surface weight
Landscapes
- Engineering & Computer Science (AREA)
- Textile Engineering (AREA)
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Manufacturing & Machinery (AREA)
- Compositions Of Macromolecular Compounds (AREA)
- Artificial Filaments (AREA)
- Fireproofing Substances (AREA)
Abstract
The invention discloses a flame-retardant elastic fabric with good moisture absorption and a preparation method thereof, wherein the fabric comprises the following raw materials in parts by weight: 30-50 parts of diphenylmethane diisocyanate, 60-70 parts of polymethyl methacrylate, 30-35 parts of polypropylene resin, 8-15 parts of p-cresol, 3-5 parts of a flame retardant and 5-8 parts of sodium dodecyl benzene sulfonate; the intermediate 6 is reacted with hydroxylamine hydrochloride to obtain an intermediate 7, the intermediate 7 is further processed to obtain an intermediate 8, the intermediate 8 and cyanuric chloride are subjected to temperature control, so that the intermediate 8 is reacted with three chlorine atom sites on the cyanuric chloride to obtain the flame retardant, the flame retardant contains a large amount of oxyacid of phosphorus, the oxyacid of phosphorus catalyzes a hydroxyl-containing compound to dehydrate into carbon, and a coke layer is generated on the surface of the heat insulation material and can insulate oxygen and heat to extinguish flame, so that the flame retardant effect of the fabric is improved.
Description
Technical Field
The invention relates to the technical field of fabric preparation, in particular to a flame-retardant elastic fabric with good hygroscopicity and a preparation method thereof.
Background
Along with the development of economic technology, the living standard of people is greatly improved, in the fashion age, the dressing requirements of people are stricter at one point, the clothes are made of fabric, the fabric is used for making the clothes, the fabric is one of three elements of the clothes, the fabric can explain the style and the characteristics of the clothes and directly control the expression effects of the color and the shape of the clothes, but the traditional fabric is single in function and only plays a role in beauty and comfort, the requirements of the fabric of the clothes at present are more and more rigorous, and the traditional fabric needs to be further optimized and improved to be more perfect and practical.
The existing flame-retardant elastic fabric has a good moisture absorption effect, but the flame-retardant effect is poor, the flame extinguishing time is long, and the burning rate of the fabric is high.
Disclosure of Invention
The invention aims to provide a flame-retardant elastic fabric with good moisture absorption and a preparation method thereof.
The technical problems to be solved by the invention are as follows:
the existing flame-retardant elastic fabric has a good moisture absorption effect, but the flame-retardant effect is poor, the flame extinguishing time is long, and the burning rate of the fabric is high.
The purpose of the invention can be realized by the following technical scheme:
the flame-retardant elastic fabric with good moisture absorption comprises the following raw materials in parts by weight: 30-50 parts of diphenylmethane diisocyanate, 60-70 parts of polymethyl methacrylate, 30-35 parts of polypropylene resin, 8-15 parts of p-cresol, 3-5 parts of a flame retardant and 5-8 parts of sodium dodecyl benzene sulfonate;
the flame-retardant elastic fabric is prepared by the following steps:
step S1: adding diphenylmethane diisocyanate, polymethyl methacrylate, polypropylene resin and p-cresol into a stirring kettle, mixing and heating to be molten under the condition that the rotating speed is 300-500r/min, adding a flame retardant, and continuously stirring for 1-1.5h to prepare a molten material;
and step S2, extruding the molten material from a spinneret plate with the diameter of 0.01-0.015mm to prepare base fibers, and weaving the base fibers according to the warp density of 70-90 pieces/cm and the weft density of 50-60 pieces/cm to prepare the flame-retardant elastic fabric.
Further, the flame retardant is prepared by the following steps:
step A1: adding tetrahydrofuran, p-chlorotoluene and magnesium powder into a reaction kettle, stirring for 0.3-0.5h under the condition that the rotation speed is 300-25 ℃ and the temperature is 500r/min, adding bromoethane, continuously stirring for 1-1.5h under the condition that the temperature is 30-35 ℃ to prepare a Grignard reagent, adding p-tolunitrile, tetrahydrofuran and toluene into the reaction kettle, stirring and dropwise adding the Grignard reagent under the conditions that the rotation speed is 150-200r/min and the temperature is 45-50 ℃, reacting for 4-6h, adding the reaction liquid into a sulfuric acid solution, cooling in an ice water bath, adding 2,2,6, 6-tetramethylpiperidine oxide, carrying out reflux reaction for 7-9h under the condition that the temperature is 110-120 ℃, layering to remove a water layer, washing an oil layer to be neutral by using a sodium hydroxide solution and distilled water in sequence, preparing an intermediate 1;
the reaction process is as follows:
step A2: adding the intermediate 1, nitrogen-bromosuccinimide, benzoyl peroxide and carbon tetrachloride into a reaction kettle, reacting for 8-10h at the rotation speed of 200-90 ℃ for 300r/min to obtain an intermediate 2, adding the intermediate 2, a potassium carbonate solution and tetraethylammonium bromide into the reaction kettle, and refluxing for 2-3h at the rotation speed of 150-200r/min and the temperature of 110-120 ℃ to obtain an intermediate 3;
the reaction process is as follows:
step A3: adding p-hydroxybenzoic acid, the intermediate 3 and tetrahydrofuran into a reaction kettle, stirring and dropwise adding concentrated sulfuric acid under the conditions that the rotation speed is 200-90 ℃ and the temperature is 80-90 ℃, reacting for 5-6h to obtain an intermediate 4, adding the intermediate 4, phosphorus oxychloride and tetrahydrofuran into the reaction kettle, stirring for 2-3h under the condition that the rotation speed is 500-800r/min, adding hydroquinone and aluminum trichloride, continuing to react for 5-8h to obtain an intermediate 5, adding the intermediate 5, neopentyl glycol phosphoryl chloride and toluene into the reaction kettle, refluxing for 8-10h, distilling to remove toluene, washing a substrate to be neutral, and obtaining an intermediate 6;
the reaction process is as follows:
step A4: adding the intermediate 6, hydroxylamine hydrochloride and ethanol solution into a reaction kettle, stirring and adding sodium hydroxide under the conditions of a rotation speed of 120-80 ℃ and a temperature of 25-30 ℃, reacting for 4-6h, heating to a temperature of 75-80 ℃, refluxing for 5-10min, adding hydrochloric acid solution, stirring for 5-10min to prepare an intermediate 7, dissolving the intermediate 7 in tetrahydrofuran, adding zinc powder and concentrated hydrochloric acid, reacting for 3-5h under the conditions of a rotation speed of 200-300r/min and a temperature of 40-50 ℃, cooling to a temperature of 0 ℃, adding ammonia water and sodium hydroxide solution, reacting for 30-50min under the condition of a temperature of 20-25 ℃ to prepare an intermediate 8, dissolving cyanuric chloride in acetone, adding the intermediate 8, refluxing for 5-6h at the rotation speed of 150-200r/min and the temperature of 80-90 ℃, and removing acetone to obtain the flame retardant.
The reaction process is as follows:
further, the dosage ratio of the p-chlorotoluene, the magnesium powder and the bromoethane in the step A1 is 1mol:1.2-1.3mol:5mL, the dosage ratio of the p-tolunitrile, the tetrahydrofuran, the toluene, the Grignard reagent, the sulfuric acid solution and the 2,2,6, 6-tetramethylpiperidine oxide is 5g:10mL:10mL:3mL:30mL:3.2g, the mass fraction of the sulfuric acid solution is 5%, and the mass fraction of the sodium hydroxide solution is 10%.
Further, the dosage ratio of the intermediate 1, the nitrogen-bromosuccinimide, the benzoyl peroxide and the carbon tetrachloride in the step A2 is 0.1mol:0.1mol:0.3g:200mL, the dosage ratio of the intermediate 2, the potassium carbonate solution and the tetraethylammonium bromide is 3g:80mL:2mL, and the mass fraction of the potassium carbonate solution is 15%.
Further, the dosage ratio of the p-hydroxybenzoic acid, the intermediate 3 and the concentrated sulfuric acid in the step A3 is 0.1mol:0.2mol:20mL, the mass fraction of the concentrated sulfuric acid is 95%, the dosage ratio of the intermediate 4, the phosphorus oxychloride, the hydroquinone and the aluminum trichloride is 0.1mol:0.4mol:0.4mol:3g, and the dosage ratio of the intermediate 5 and the neopentyl glycol phosphoryl chloride is 1: 4.
Further, the intermediate 6, the hydroxylamine hydrochloride, the ethanol solution, the sodium hydroxide and the hydrochloric acid solution in the step A4 are used in an amount ratio of 5g:3g:15mL:2g:8mL, the ethanol solution accounts for 80% by mass, the hydrochloric acid solution accounts for 10-13% by mass, the intermediate 7, the zinc powder, the concentrated hydrochloric acid, the ammonia water and the sodium hydroxide solution are used in an amount ratio of 0.02mol:0.2mol:15mL:25mL:60mL, the concentrated hydrochloric acid accounts for 37% by mass, the ammonia water accounts for 30% by mass, the sodium hydroxide solution accounts for 20% by mass, and the cyanuric chloride and the intermediate 8 are used in a molar ratio of 1: 3.
A preparation method of a flame-retardant elastic fabric with good hygroscopicity specifically comprises the following steps:
step S1: adding diphenylmethane diisocyanate, polymethyl methacrylate, polypropylene resin and p-cresol into a stirring kettle, mixing and heating to be molten under the condition that the rotating speed is 300-500r/min, adding a flame retardant, and continuously stirring for 1-1.5h to prepare a molten material;
and step S2, extruding the molten material from a spinneret plate with the diameter of 0.01-0.015mm to prepare base fibers, and weaving the base fibers according to the warp density of 70-90 pieces/cm and the weft density of 50-60 pieces/cm to prepare the flame-retardant elastic fabric.
The invention has the beneficial effects that: the invention prepares a flame retardant in the process of preparing a flame-retardant elastic fabric with good hygroscopicity, the flame retardant takes p-chlorotoluene as a raw material to react with magnesium powder to prepare a Grignard reagent, the Grignard reagent reacts with p-tolunitrile and is subjected to acidic hydrolysis to prepare an intermediate 1, the intermediate 1 reacts with nitrogen-bromosuccinimide to prepare an intermediate 2, the intermediate 2 is further processed to prepare an intermediate 3, the intermediate 3 reacts with p-hydroxybenzoic acid to prepare an intermediate 4, the intermediate 4 reacts with phosphorus oxychloride to prepare an intermediate 5, the intermediate 5 reacts with neopentyl glycol phosphoryl chloride to prepare an intermediate 6, the intermediate 6 reacts with hydroxylamine hydrochloride to prepare an intermediate 7, the intermediate 7 is further processed to prepare an intermediate 8, the intermediate 8 and cyanuric chloride are subjected to temperature control, the intermediate 8 and three chlorine atom sites on cyanuric chloride react to prepare the flame retardant, the flame retardant contains a large amount of oxyacid of phosphorus, the oxyacid of phosphorus catalyzes a hydroxyl-containing compound to dehydrate into carbon, and a coke layer is generated on the surface of the heat insulation material, and the coke layer can insulate oxygen and heat and further extinguish flame, so that the flame retardant effect of the fabric is improved.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1
The flame-retardant elastic fabric with good moisture absorption comprises the following raw materials in parts by weight: 30 parts of diphenylmethane diisocyanate, 60 parts of polymethyl methacrylate, 30 parts of polypropylene resin, 8 parts of p-cresol, 3 parts of a flame retardant and 5 parts of sodium dodecyl benzene sulfonate;
the flame-retardant elastic fabric is prepared by the following steps:
step S1: adding diphenylmethane diisocyanate, polymethyl methacrylate, polypropylene resin and p-cresol into a stirring kettle, mixing and heating to be molten under the condition that the rotating speed is 300r/min, adding a flame retardant, and continuously stirring for 1h to prepare a molten material;
and step S2, extruding the molten material from a spinneret plate with the diameter of 0.01mm to prepare base fibers, and spinning the base fibers according to the warp density of 70 pieces/cm and the weft density of 50 pieces/cm to prepare the flame-retardant elastic fabric.
The flame retardant is prepared by the following steps:
step A1: adding tetrahydrofuran, p-chlorotoluene and magnesium powder into a reaction kettle, stirring for 0.3h at the rotation speed of 300r/min and the temperature of 20 ℃, adding bromoethane, continuously stirring for 1h at the temperature of 30 ℃ to prepare a Grignard reagent, adding p-tolunitrile, tetrahydrofuran and toluene into the reaction kettle, stirring and dropwise adding the Grignard reagent at the rotation speed of 150r/min and the temperature of 45 ℃, reacting for 4h to prepare an intermediate 1, adding the intermediate 1 into a sulfuric acid solution, cooling in an ice water bath, adding 2,2,6, 6-tetramethylpiperidine oxide, carrying out reflux reaction for 7h at the temperature of 110 ℃, layering to remove a water layer, and washing an oil layer to be neutral by using a sodium hydroxide solution and distilled water in sequence to prepare the intermediate 1;
step A2: adding the intermediate 1, nitrogen-bromosuccinimide, benzoyl peroxide and carbon tetrachloride into a reaction kettle, reacting for 8 hours at the rotation speed of 200r/min and the temperature of 80 ℃ to obtain an intermediate 2, adding the intermediate 2, a potassium carbonate solution and tetraethylammonium bromide into the reaction kettle, and refluxing for 2 hours at the rotation speed of 150r/min and the temperature of 110 ℃ to obtain an intermediate 3;
step A3: adding p-hydroxybenzoic acid, the intermediate 3 and tetrahydrofuran into a reaction kettle, stirring and dropwise adding concentrated sulfuric acid under the conditions of the rotating speed of 200r/min and the temperature of 80 ℃ to react for 5 hours to obtain an intermediate 4, adding the intermediate 4, phosphorus oxychloride and tetrahydrofuran into the reaction kettle, stirring for 2 hours under the condition of the rotating speed of 500r/min, adding phenol and aluminum trichloride, continuing to react for 5 hours to obtain an intermediate 5, adding the intermediate 5, neopentyl glycol phosphoryl chloride and toluene into the reaction kettle, refluxing for 8 hours, distilling to remove toluene, washing a substrate with water to be neutral, and preparing an intermediate 6;
step A4: adding the intermediate 6, hydroxylamine hydrochloride and ethanol solution into a reaction kettle, stirring and adding sodium hydroxide under the conditions of the rotating speed of 120r/min and the temperature of 25 ℃, reacting for 4 hours, heating to 75 deg.C, refluxing for 5min, adding hydrochloric acid solution, stirring for 5min to obtain intermediate 7, dissolving intermediate 7 in tetrahydrofuran, adding zinc powder and concentrated hydrochloric acid, reacting for 3h at the rotation speed of 200r/min and the temperature of 40 ℃, cooling to the temperature of 0 ℃, adding ammonia water and sodium hydroxide solution, reacting at 20 deg.C for 30min to obtain intermediate 8, dissolving cyanuric chloride in acetone, adding intermediate 8, refluxing for 5h at the rotation speed of 150r/min and the temperature of 80 ℃, and removing acetone to obtain the flame retardant.
Example 2
The flame-retardant elastic fabric with good moisture absorption comprises the following raw materials in parts by weight: 40 parts of diphenylmethane diisocyanate, 65 parts of polymethyl methacrylate, 33 parts of polypropylene resin, 10 parts of p-cresol, 4 parts of a flame retardant and 6 parts of sodium dodecyl benzene sulfonate;
the flame-retardant elastic fabric is prepared by the following steps:
step S1: adding diphenylmethane diisocyanate, polymethyl methacrylate, polypropylene resin and p-cresol into a stirring kettle, mixing and heating to be molten under the condition that the rotating speed is 300r/min, adding a flame retardant, and continuously stirring for 1.5 hours to prepare a molten material;
and step S2, extruding the molten material from a spinneret plate with the diameter of 0.01mm to prepare base fibers, and spinning the base fibers according to the warp density of 90 pieces/cm and the weft density of 50 pieces/cm to prepare the flame-retardant elastic fabric.
Example 3
The flame-retardant elastic fabric with good moisture absorption comprises the following raw materials in parts by weight: 50 parts of diphenylmethane diisocyanate, 70 parts of polymethyl methacrylate, 35 parts of polypropylene resin, 15 parts of paracresol, 5 parts of flame retardant and 8 parts of sodium dodecyl benzene sulfonate;
the flame-retardant elastic fabric is prepared by the following steps:
step S1: adding diphenylmethane diisocyanate, polymethyl methacrylate, polypropylene resin and p-cresol into a stirring kettle, mixing and heating to be molten under the condition that the rotating speed is 500r/min, adding a flame retardant, and continuously stirring for 1.5 hours to prepare a molten material;
and step S2, extruding the molten material from a spinneret plate with the diameter of 0.015mm to prepare base fibers, and weaving the base fibers according to the warp density of 90 pieces/cm and the weft density of 60 pieces/cm to prepare the flame-retardant elastic fabric.
Comparative example
The comparative example is a common flame-retardant fabric in the market.
The results of performance tests on the flame retardant fabrics prepared in examples 1 to 3 and comparative example are shown in table 1 below;
the flame-retardant fabrics obtained in examples 1 to 3 and comparative example were cut into strips of 50cm long and 5cm wide, and were burned from the bottom, and the flame-out time and the fabric combustion rate were recorded.
TABLE 1
| Example 1 | Example 2 | Example 3 | Comparative example | |
| Time to flame-out | 2.5s | 3.2s | 2.7s | 5.8s |
| Burning rate of the fabric | 12％ | 15％ | 13％ | 35％ |
From the above table 1, it can be seen that the flame extinguishing time of the flame-retardant fabric prepared in the examples 1-3 is 2.5-3.2s, and the combustion rate of the fabric is 12-15%, while the flame extinguishing time of the flame-retardant fabric prepared in the comparative example is 5.8s, and the combustion rate of the fabric is 35%, so that the flame-retardant fabric has a good flame-retardant effect.
The foregoing is merely exemplary and illustrative of the principles of the present invention and various modifications, additions and substitutions of the specific embodiments described herein may be made by those skilled in the art without departing from the principles of the present invention or exceeding the scope of the claims set forth herein.
Claims (7)
1. The flame-retardant elastic fabric with good moisture absorption is characterized in that: the feed comprises the following raw materials in parts by weight: 30-50 parts of diphenylmethane diisocyanate, 60-70 parts of polymethyl methacrylate, 30-35 parts of polypropylene resin, 8-15 parts of p-cresol, 3-5 parts of a flame retardant and 5-8 parts of sodium dodecyl benzene sulfonate;
the flame-retardant elastic fabric is prepared by the following steps:
step S1: adding diphenylmethane diisocyanate, polymethyl methacrylate, polypropylene resin and p-cresol into a stirring kettle, mixing and heating to be molten under the condition that the rotating speed is 300-500r/min, adding a flame retardant, and continuously stirring for 1-1.5h to prepare a molten material;
and step S2, extruding the molten material from a spinneret plate with the diameter of 0.01-0.015mm to prepare base fibers, and weaving the base fibers according to the warp density of 70-90 pieces/cm and the weft density of 50-60 pieces/cm to prepare the flame-retardant elastic fabric.
2. The flame-retardant elastic fabric with good moisture absorption performance as claimed in claim 1, wherein the flame-retardant elastic fabric is characterized in that: the flame retardant is prepared by the following steps:
step A1: adding tetrahydrofuran, p-chlorotoluene and magnesium powder into a reaction kettle, stirring for 0.3-0.5h under the condition that the rotation speed is 300-25 ℃ and the temperature is 500r/min, adding bromoethane, continuously stirring for 1-1.5h under the condition that the temperature is 30-35 ℃ to prepare a Grignard reagent, adding p-tolunitrile, tetrahydrofuran and toluene into the reaction kettle, stirring and dropwise adding the Grignard reagent under the conditions that the rotation speed is 150-200r/min and the temperature is 45-50 ℃, reacting for 4-6h, adding the reaction liquid into a sulfuric acid solution, cooling in an ice water bath, adding 2,2,6, 6-tetramethylpiperidine oxide, carrying out reflux reaction for 7-9h under the condition that the temperature is 110-120 ℃, layering to remove a water layer, washing an oil layer to be neutral by using a sodium hydroxide solution and distilled water in sequence, preparing an intermediate 1;
step A2: adding the intermediate 1, nitrogen-bromosuccinimide, benzoyl peroxide and carbon tetrachloride into a reaction kettle, reacting for 8-10h at the rotation speed of 200-90 ℃ for 300r/min to obtain an intermediate 2, adding the intermediate 2, a potassium carbonate solution and tetraethylammonium bromide into the reaction kettle, and refluxing for 2-3h at the rotation speed of 150-200r/min and the temperature of 110-120 ℃ to obtain an intermediate 3;
step A3: adding p-hydroxybenzoic acid, the intermediate 3 and tetrahydrofuran into a reaction kettle, stirring and dropwise adding concentrated sulfuric acid under the conditions that the rotation speed is 200-90 ℃ and the temperature is 80-90 ℃, reacting for 5-6h to obtain an intermediate 4, adding the intermediate 4, phosphorus oxychloride and tetrahydrofuran into the reaction kettle, stirring for 2-3h under the condition that the rotation speed is 500-800r/min, adding hydroquinone and aluminum trichloride, continuing to react for 5-8h to obtain an intermediate 5, adding the intermediate 5, neopentyl glycol phosphoryl chloride and toluene into the reaction kettle, refluxing for 8-10h, distilling to remove toluene, washing a substrate to be neutral, and obtaining an intermediate 6;
step A4: adding the intermediate 6, hydroxylamine hydrochloride and ethanol solution into a reaction kettle, stirring and adding sodium hydroxide under the conditions of a rotation speed of 120-80 ℃ and a temperature of 25-30 ℃, reacting for 4-6h, heating to a temperature of 75-80 ℃, refluxing for 5-10min, adding hydrochloric acid solution, stirring for 5-10min to prepare an intermediate 7, dissolving the intermediate 7 in tetrahydrofuran, adding zinc powder and concentrated hydrochloric acid, reacting for 3-5h under the conditions of a rotation speed of 200-300r/min and a temperature of 40-50 ℃, cooling to a temperature of 0 ℃, adding ammonia water and sodium hydroxide solution, reacting for 30-50min under the condition of a temperature of 20-25 ℃ to prepare an intermediate 8, dissolving cyanuric chloride in acetone, adding the intermediate 8, refluxing for 5-6h at the rotation speed of 150-200r/min and the temperature of 80-90 ℃, and removing acetone to obtain the flame retardant.
3. The flame-retardant elastic fabric with good moisture absorption performance as claimed in claim 2, wherein: the dosage ratio of the p-chlorotoluene, the magnesium powder and the bromoethane in the step A1 is 1mol:1.2-1.3mol:5mL, the dosage ratio of the p-tolunitrile, the tetrahydrofuran, the toluene, the Grignard reagent, the sulfuric acid solution and the 2,2,6, 6-tetramethylpiperidine oxide is 5g:10mL:10mL:3mL:30mL:3.2g, the mass fraction of the sulfuric acid solution is 5%, and the mass fraction of the sodium hydroxide solution is 10%.
4. The flame-retardant elastic fabric with good moisture absorption performance as claimed in claim 2, wherein: the dosage ratio of the intermediate 1, the nitrogen-bromosuccinimide, the benzoyl peroxide and the carbon tetrachloride in the step A2 is 0.1mol:0.1mol:0.3g:200mL, the dosage ratio of the intermediate 2, the potassium carbonate solution and the tetraethylammonium bromide is 3g:80mL:2mL, and the mass fraction of the potassium carbonate solution is 15%.
5. The flame-retardant elastic fabric with good moisture absorption performance as claimed in claim 2, wherein: the dosage ratio of the p-hydroxybenzoic acid, the intermediate 3 and the concentrated sulfuric acid in the step A3 is 0.1mol:0.2mol:20mL, the mass fraction of the concentrated sulfuric acid is 95%, the dosage ratio of the intermediate 4, the phosphorus oxychloride, the hydroquinone and the aluminum trichloride is 0.1mol:0.4mol:0.4mol:3g, and the dosage ratio of the intermediate 5 and the neopentyl glycol phosphoryl chloride is 1: 4.
6. The flame-retardant elastic fabric with good moisture absorption performance as claimed in claim 2, wherein: the intermediate 6, the hydroxylamine hydrochloride, the ethanol solution, the sodium hydroxide and the hydrochloric acid solution are used in the step A4, the dosage ratio of the intermediate 6, the hydroxylamine hydrochloride, the ethanol solution is 5g:3g:15mL:2g:8mL, the mass fraction of the ethanol solution is 80%, the mass fraction of the hydrochloric acid solution is 10-13%, the dosage ratio of the intermediate 7, the zinc powder, the concentrated hydrochloric acid, the ammonia water and the sodium hydroxide solution is 0.02mol:0.2mol:15mL:25mL:60mL, the mass fraction of the concentrated hydrochloric acid is 37%, the mass fraction of the ammonia water is 30%, the mass fraction of the sodium hydroxide solution is 20%, and the dosage molar ratio of the cyanuric chloride to the intermediate 8 is 1: 3.
7. The flame-retardant elastic fabric with good moisture absorption property as claimed in claim 2, wherein the flame-retardant elastic fabric is characterized in that: the method specifically comprises the following steps:
step S1: adding diphenylmethane diisocyanate, polymethyl methacrylate, polypropylene resin and p-cresol into a stirring kettle, mixing and heating to be molten under the condition that the rotating speed is 300-500r/min, adding a flame retardant, and continuously stirring for 1-1.5h to prepare a molten material;
and step S2, extruding the molten material from a spinneret plate with the diameter of 0.01-0.015mm to prepare base fibers, and weaving the base fibers according to the warp density of 70-90 pieces/cm and the weft density of 50-60 pieces/cm to prepare the flame-retardant elastic fabric.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113978053A (en) * | 2021-12-14 | 2022-01-28 | 常熟新常泰汽车内饰科技有限公司 | Environment-friendly wear-resistant automobile carpet and preparation method thereof |
| CN116987247A (en) * | 2023-09-25 | 2023-11-03 | 世京(德州)新型材料科技有限公司 | Magnesium-aluminum hydrotalcite composite material and preparation method thereof |
-
2021
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113978053A (en) * | 2021-12-14 | 2022-01-28 | 常熟新常泰汽车内饰科技有限公司 | Environment-friendly wear-resistant automobile carpet and preparation method thereof |
| CN113978053B (en) * | 2021-12-14 | 2023-07-25 | 常熟新常泰汽车内饰科技有限公司 | Environment-friendly wear-resistant automobile carpet and preparation method thereof |
| CN116987247A (en) * | 2023-09-25 | 2023-11-03 | 世京(德州)新型材料科技有限公司 | Magnesium-aluminum hydrotalcite composite material and preparation method thereof |
| CN116987247B (en) * | 2023-09-25 | 2023-12-08 | 世京(德州)新型材料科技有限公司 | Magnesium-aluminum hydrotalcite composite material and preparation method thereof |
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