CN117863699A - Flame-retardant carpet fabric and preparation method thereof - Google Patents
Flame-retardant carpet fabric and preparation method thereof Download PDFInfo
- Publication number
- CN117863699A CN117863699A CN202310222881.0A CN202310222881A CN117863699A CN 117863699 A CN117863699 A CN 117863699A CN 202310222881 A CN202310222881 A CN 202310222881A CN 117863699 A CN117863699 A CN 117863699A
- Authority
- CN
- China
- Prior art keywords
- flame
- base cloth
- quaternary ammonium
- hours
- heating
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
- 239000004744 fabric Substances 0.000 title claims abstract description 89
- RNFJDJUURJAICM-UHFFFAOYSA-N 2,2,4,4,6,6-hexaphenoxy-1,3,5-triaza-2$l^{5},4$l^{5},6$l^{5}-triphosphacyclohexa-1,3,5-triene Chemical compound N=1P(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP=1(OC=1C=CC=CC=1)OC1=CC=CC=C1 RNFJDJUURJAICM-UHFFFAOYSA-N 0.000 title claims abstract description 76
- 239000003063 flame retardant Substances 0.000 title claims abstract description 76
- 238000002360 preparation method Methods 0.000 title claims abstract description 12
- 238000004519 manufacturing process Methods 0.000 title description 2
- -1 imidazoline quaternary ammonium copper complex Chemical class 0.000 claims abstract description 100
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 70
- PAYRUJLWNCNPSJ-UHFFFAOYSA-N Aniline Chemical compound NC1=CC=CC=C1 PAYRUJLWNCNPSJ-UHFFFAOYSA-N 0.000 claims abstract description 64
- 239000002585 base Substances 0.000 claims abstract description 57
- 239000004814 polyurethane Substances 0.000 claims abstract description 55
- 229920002635 polyurethane Polymers 0.000 claims abstract description 54
- UMGDCJDMYOKAJW-UHFFFAOYSA-N thiourea Chemical compound NC(N)=S UMGDCJDMYOKAJW-UHFFFAOYSA-N 0.000 claims abstract description 46
- 229920001296 polysiloxane Polymers 0.000 claims abstract description 40
- 239000000835 fiber Substances 0.000 claims abstract description 39
- 229920002239 polyacrylonitrile Polymers 0.000 claims abstract description 38
- 239000003513 alkali Substances 0.000 claims abstract description 26
- 239000002608 ionic liquid Substances 0.000 claims abstract description 26
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Natural products NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims abstract description 23
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims abstract description 22
- 239000001257 hydrogen Substances 0.000 claims abstract description 22
- 229910052739 hydrogen Inorganic materials 0.000 claims abstract description 22
- 229920002545 silicone oil Polymers 0.000 claims abstract description 22
- NIXOWILDQLNWCW-UHFFFAOYSA-N acrylic acid group Chemical group C(C=C)(=O)O NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 claims abstract description 20
- 229920002972 Acrylic fiber Polymers 0.000 claims abstract description 12
- 239000013530 defoamer Substances 0.000 claims abstract description 12
- 229920002678 cellulose Polymers 0.000 claims abstract description 9
- 239000001913 cellulose Substances 0.000 claims abstract description 9
- 230000000379 polymerizing effect Effects 0.000 claims abstract description 4
- 238000010438 heat treatment Methods 0.000 claims description 63
- 238000003756 stirring Methods 0.000 claims description 60
- 238000002156 mixing Methods 0.000 claims description 53
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 46
- 238000006243 chemical reaction Methods 0.000 claims description 44
- 235000021355 Stearic acid Nutrition 0.000 claims description 27
- QIQXTHQIDYTFRH-UHFFFAOYSA-N octadecanoic acid Chemical compound CCCCCCCCCCCCCCCCCC(O)=O QIQXTHQIDYTFRH-UHFFFAOYSA-N 0.000 claims description 27
- OQCDKBAXFALNLD-UHFFFAOYSA-N octadecanoic acid Natural products CCCCCCCC(C)CCCCCCCCC(O)=O OQCDKBAXFALNLD-UHFFFAOYSA-N 0.000 claims description 27
- 239000008117 stearic acid Substances 0.000 claims description 27
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 24
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 24
- 239000008367 deionised water Substances 0.000 claims description 23
- 229910021641 deionized water Inorganic materials 0.000 claims description 23
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 21
- 238000000034 method Methods 0.000 claims description 21
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims description 20
- 238000005406 washing Methods 0.000 claims description 17
- WYURNTSHIVDZCO-UHFFFAOYSA-N Tetrahydrofuran Chemical compound C1CCOC1 WYURNTSHIVDZCO-UHFFFAOYSA-N 0.000 claims description 16
- 230000001276 controlling effect Effects 0.000 claims description 16
- KPUWHANPEXNPJT-UHFFFAOYSA-N disiloxane Chemical class [SiH3]O[SiH3] KPUWHANPEXNPJT-UHFFFAOYSA-N 0.000 claims description 16
- 239000000178 monomer Substances 0.000 claims description 16
- 238000003825 pressing Methods 0.000 claims description 16
- 238000002390 rotary evaporation Methods 0.000 claims description 16
- 238000001914 filtration Methods 0.000 claims description 15
- 239000000203 mixture Substances 0.000 claims description 15
- ROOXNKNUYICQNP-UHFFFAOYSA-N ammonium persulfate Chemical compound [NH4+].[NH4+].[O-]S(=O)(=O)OOS([O-])(=O)=O ROOXNKNUYICQNP-UHFFFAOYSA-N 0.000 claims description 14
- 239000002518 antifoaming agent Substances 0.000 claims description 12
- RPNUMPOLZDHAAY-UHFFFAOYSA-N Diethylenetriamine Chemical compound NCCNCCN RPNUMPOLZDHAAY-UHFFFAOYSA-N 0.000 claims description 11
- KCXMKQUNVWSEMD-UHFFFAOYSA-N benzyl chloride Chemical compound ClCC1=CC=CC=C1 KCXMKQUNVWSEMD-UHFFFAOYSA-N 0.000 claims description 11
- 229940073608 benzyl chloride Drugs 0.000 claims description 11
- NWFNSTOSIVLCJA-UHFFFAOYSA-L copper;diacetate;hydrate Chemical compound O.[Cu+2].CC([O-])=O.CC([O-])=O NWFNSTOSIVLCJA-UHFFFAOYSA-L 0.000 claims description 11
- 229920002503 polyoxyethylene-polyoxypropylene Polymers 0.000 claims description 10
- 238000009987 spinning Methods 0.000 claims description 10
- 238000009941 weaving Methods 0.000 claims description 9
- UIIMBOGNXHQVGW-DEQYMQKBSA-M Sodium bicarbonate-14C Chemical compound [Na+].O[14C]([O-])=O UIIMBOGNXHQVGW-DEQYMQKBSA-M 0.000 claims description 8
- 238000001816 cooling Methods 0.000 claims description 8
- 238000001035 drying Methods 0.000 claims description 8
- 239000012299 nitrogen atmosphere Substances 0.000 claims description 8
- 238000010992 reflux Methods 0.000 claims description 8
- 230000001105 regulatory effect Effects 0.000 claims description 8
- YLQBMQCUIZJEEH-UHFFFAOYSA-N tetrahydrofuran Natural products C=1C=COC=1 YLQBMQCUIZJEEH-UHFFFAOYSA-N 0.000 claims description 8
- 238000001291 vacuum drying Methods 0.000 claims description 8
- KAIPKTYOBMEXRR-UHFFFAOYSA-N 1-butyl-3-methyl-2h-imidazole Chemical compound CCCCN1CN(C)C=C1 KAIPKTYOBMEXRR-UHFFFAOYSA-N 0.000 claims description 7
- 229920000742 Cotton Polymers 0.000 claims description 7
- 229910001870 ammonium persulfate Inorganic materials 0.000 claims description 7
- 239000003999 initiator Substances 0.000 claims description 7
- 238000007112 amidation reaction Methods 0.000 claims description 3
- 150000001412 amines Chemical class 0.000 claims description 3
- 239000004205 dimethyl polysiloxane Substances 0.000 claims description 3
- 238000010030 laminating Methods 0.000 claims description 3
- 229920000435 poly(dimethylsiloxane) Polymers 0.000 claims description 3
- 238000005956 quaternization reaction Methods 0.000 claims description 3
- 239000002994 raw material Substances 0.000 claims description 3
- 238000007363 ring formation reaction Methods 0.000 claims description 3
- 239000011229 interlayer Substances 0.000 abstract description 5
- 125000003277 amino group Chemical group 0.000 abstract description 2
- 230000000052 comparative effect Effects 0.000 description 9
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 2
- 229920005610 lignin Polymers 0.000 description 2
- 229920000767 polyaniline Polymers 0.000 description 2
- 230000003746 surface roughness Effects 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 238000002485 combustion reaction Methods 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 150000004699 copper complex Chemical class 0.000 description 1
- 238000004132 cross linking Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000011065 in-situ storage Methods 0.000 description 1
- 239000010410 layer Substances 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000002715 modification method Methods 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 230000035699 permeability Effects 0.000 description 1
- 238000006116 polymerization reaction Methods 0.000 description 1
- 229920006306 polyurethane fiber Polymers 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
Landscapes
- Treatments For Attaching Organic Compounds To Fibrous Goods (AREA)
Abstract
The invention discloses a flame-retardant carpet fabric and a preparation method thereof, and relates to the technical field of fabrics. When the fabric for the flame-retardant carpet is prepared, the polyurethane base cloth and the acrylic base cloth are pressed together to prepare the flame-retardant carpet; the polyurethane base cloth comprises polyurethane, self-made flame retardant, hydrogen-containing silicone oil, lignocellulose, defoamer and ethanol; the acrylic base cloth is woven by modified polyacrylonitrile fibers; the self-made flame retardant is prepared by reacting thiourea-based imidazoline quaternary ammonium copper complex with amino-terminated hyperbranched polysiloxane, so that the polyurethane base cloth has excellent flame retardance; the modified polyacrylonitrile fiber is prepared by polymerizing aniline on the surface of the polyacrylonitrile fiber, then performing alkali treatment, and then performing post-treatment by using an ionic liquid with cellulose, so that the tensile strength of the acrylic fiber interlayer is enhanced; and after the polyurethane base cloth and the acrylic base cloth are pressed, amino groups on the polyurethane base cloth can react with a cellulose film of the acrylic interlayer, so that the mechanical property of the fabric for the flame-retardant carpet is enhanced.
Description
Technical Field
The invention relates to the technical field of fabrics, in particular to a flame-retardant carpet fabric and a preparation method thereof.
Background
The flame-retardant modification method of the fabric can be divided into two main types: one is a pre-spinning method, namely adding a flame retardant in the spinning process, and weaving flame-retardant fibers into flame-retardant fabric, wherein the fabric prepared by the method has good flame-retardant durability, and can still keep the flame retardance close to that of the original fabric after being subjected to multiple water washing; the other type is a post-finishing method, namely, the flame retardant is applied to the surface of the fabric by physical coating, chemical grafting and other methods when the fabric is manufactured, the method has low cost and quick response, however, the poor washing fastness is a common problem of the post-finishing functional fabric; in addition, the hand feeling, style, air permeability and other aspects of the fabric after finishing are often affected.
Therefore, the invention approximates to adding the flame retardant in the preparation process, and also composites polyurethane and acrylic fibers to prepare the flame-retardant carpet fabric with excellent flame retardant property and good mechanical property.
Disclosure of Invention
The invention aims to provide a flame-retardant carpet fabric and a preparation method thereof, which are used for solving the problems in the background technology.
In order to solve the technical problems, the invention provides the following technical scheme: the fabric for the flame-retardant carpet is prepared by laminating polyurethane base cloth and acrylic base cloth; the polyurethane base cloth comprises polyurethane, self-made flame retardant, hydrogen-containing silicone oil, lignocellulose, defoamer and ethanol; the acrylic base cloth is woven by modified polyacrylonitrile fibers; the defoaming agent is one or more of polydimethylsiloxane, polyoxyethylene polyoxypropylene pentaerythritol ether and polyoxyethylene polyoxypropylene alcohol amine ether.
Preferably, the self-made flame retardant is prepared by reacting thiourea-based imidazoline quaternary ammonium copper complex with amino-terminated hyperbranched polysiloxane; the thioureido imidazoline quaternary ammonium copper complex is prepared by reacting thioureido imidazoline quaternary ammonium salt with copper acetate-hydrate.
Preferably, the thioureido imidazoline quaternary ammonium salt is prepared by taking stearic acid and diethylenetriamine as reaction raw materials, carrying out amidation reaction and cyclization reaction, then carrying out quaternization reaction with benzyl chloride, and finally introducing thiourea.
Preferably, the modified polyacrylonitrile fiber is prepared by polymerizing aniline on the surface of the polyacrylonitrile fiber, then performing alkali treatment, and then performing post-treatment by using an ionic liquid with cellulose.
Preferably, the preparation method of the flame-retardant carpet fabric comprises the following specific steps:
(1) Mixing hyperbranched polysiloxane and deionized water according to a mass ratio of 1:1.3-1:1.6, uniformly stirring, regulating pH to 5 by hydrochloric acid, heating to 50-55 ℃, reacting for 4-6 hours, performing rotary evaporation, and vacuum drying at 55-65 ℃ to obtain amino-terminated hyperbranched polysiloxane;
(2) Mixing thioureido imidazoline quaternary ammonium salt and ethanol according to the mass ratio of 1:25-1:50, stirring until the mixture is dissolved, adding copper acetate-hydrate with the mass of 0.4-0.6 times that of the thioureido imidazoline quaternary ammonium salt, stirring at 100-200 rpm for reaction for 20-40 min, heating to 110-120 ℃, carrying out reflux reaction for 24h, filtering, washing with absolute ethanol and deionized water for 3-5 times, and drying until the weight is constant, thus obtaining the thioureido imidazoline quaternary ammonium copper complex;
(3) Mixing the amino-terminated hyperbranched polysiloxane and the thiourea-based imidazoline quaternary ammonium copper complex in a mass ratio of 50:1-80:3, and placing the mixture in an internal mixer for banburying for 5-8 hours to prepare a self-made flame retardant;
(4) Placing polyurethane into a reaction kettle, preheating for 5-8 min at 70-80 ℃, sequentially adding a self-made flame retardant, hydrogen-containing silicone oil, lignocellulose, a defoaming agent and ethanol, heating to 100-120 ℃, preserving heat for 30-50 min, and transferring to a loom to obtain polyurethane base cloth;
(5) Mixing aniline and hydrochloric acid with the mass fraction of 2-4% according to the mass ratio of 1:8-1:10, uniformly stirring to obtain an aniline solution, immersing polyacrylonitrile fibers in the aniline solution, stirring at 100-200 rpm, dropwise adding ammonium persulfate serving as an initiator with the mass of 0.03-0.06 times of that of the aniline at the speed of 1-2 ml/min, continuously stirring to react until the color is changed into dark green, continuously reacting for 2-3 h, and fishing out to perform alkali treatment and ionic liquid aftertreatment to obtain modified polyacrylonitrile fibers; after double twisting, spinning and weaving, the yarn with the gram weight of 200 to 400g/m is prepared 2 Acrylic base cloth;
(6) Arranging the polyurethane base cloth and the acrylic fiber base in a pressing machine, and pressing for 2-4 min at 110-120 ℃ to obtain the flame-retardant carpet fabric.
Preferably, in the step (1): the preparation method of the hyperbranched polysiloxane comprises the following steps: uniformly mixing and stirring siloxane monomers, methanol and tetrahydrofuran according to the mass ratio of 1:5:15-1:5:20, heating to 52-55 ℃, preserving heat for 10-20 min, dropwise adding hydrochloric acid with the mass fraction of 0.5-1.5% of the siloxane monomers at the rate of 3-5 ml/min into the mixture, continuously reacting for 4-6 h, adjusting the pH to 6.8-7.2 by using sodium bicarbonate, and performing rotary evaporation at the temperature of 55-65 ℃ to obtain the hyperbranched polysiloxane.
Preferably, in the step (2): the preparation method of the thioureido imidazoline quaternary ammonium salt comprises the following steps: mixing stearic acid and diethylenetriamine according to a mass ratio of 1:1-1:1.2, heating to 150-160 ℃, controlling the reaction pressure to 8-8.3 kPa, reacting for 3-5 hours, continuously heating to 190-200 ℃, controlling the pressure to 5.05-5.07 kPa, transferring to a nitrogen atmosphere, continuously reacting for 3-5 hours, dropwise adding benzyl chloride with a mass of 0.2-0.4 times of stearic acid at a speed of 1-2 ml/min, transferring to an oil bath, reacting for 2-3 hours at a temperature of 105-115 ℃, cooling to room temperature, adding thiourea with a mass of 1.1-1.3 times of stearic acid, and continuously reacting for 1-2 hours to obtain the thioureido imidazoline quaternary ammonium salt.
Preferably, in the step (4): the mass ratio of the polyurethane to the self-made flame retardant to the hydrogen-containing silicone oil to the lignocellulose to the defoamer to the ethanol is 7:1:0.5:1:0.002:2-9:1.5:0.8:2:0.012:3.
Preferably, in the step (5): the alkali treatment process comprises the following steps: immersing in sodium hydroxide solution with the mass fraction of 4-6%, heating to 70-80 ℃, treating for 20-30 min, and washing with deionized water for 2-3 min.
Preferably, in the step (5): the post-treatment process of the ionic liquid comprises the following steps: mixing cotton fiber and ionic liquid chloridized 1-butyl-3-methylimidazole according to a mass ratio of 1:10-1:20, heating to 90-110 ℃, stirring at 100-200 rpm for reaction for 5-6 hours, filtering, immersing the polyacrylonitrile fiber subjected to alkali treatment, and standing for 8-12 hours.
Compared with the prior art, the invention has the following beneficial effects:
the prepared fabric for the flame-retardant carpet is prepared by laminating polyurethane base cloth and acrylic base cloth; the polyurethane base cloth comprises polyurethane, self-made flame retardant, hydrogen-containing silicone oil, lignocellulose, defoamer and ethanol; the acrylic base cloth is woven by modified polyacrylonitrile fibers;
the self-made flame retardant is prepared by reacting thiourea-based imidazoline quaternary ammonium copper complex and amino-terminated hyperbranched polysiloxane; stearic acid and diethylenetriamine are used as reaction raw materials, after amidation reaction and cyclization reaction, the reaction is performed with benzyl chloride for quaternization, finally thiourea is introduced to prepare thiourea imidazoline quaternary ammonium salt, the thiourea imidazoline quaternary ammonium salt reacts with copper acetate-hydrate to synthesize thiourea imidazoline quaternary ammonium copper complex, the copper complex can enter a silica cross-linking network structure of amino-terminated hyperbranched polysiloxane, the thiourea imidazoline quaternary ammonium salt can be adsorbed in the network structure, a continuous compact carbon layer can be formed during combustion, and a self-made flame retardant is added into polyurethane, so that polyurethane base cloth has excellent flame retardance;
the modified polyacrylonitrile fiber is prepared by polymerizing aniline on the surface of the polyacrylonitrile fiber, then performing alkali treatment, and then performing post-treatment by using an ionic liquid with cellulose; in-situ polymerization is carried out on the surface of the polyacrylonitrile fiber to form polyaniline, the antistatic property of the acrylic fiber interlayer is enhanced, then the polyaniline on the surface is treated by alkali to form the polyacrylonitrile fiber with a surface roughness structure, finally the ionic liquid is used for carrying out post-treatment, a cellulose film is generated on the polyacrylonitrile fiber with the surface roughness, and the tensile strength of the acrylic fiber interlayer is enhanced; and after the polyurethane base cloth and the acrylic base cloth are pressed, amino groups on the polyurethane base cloth can react with a cellulose film of the acrylic interlayer, so that the mechanical property of the fabric for the flame-retardant carpet is enhanced.
Detailed Description
The technical solutions of the embodiments of the present invention will be clearly and completely described below in conjunction with the embodiments of the present invention, and it is apparent that the described embodiments are only some embodiments of the present invention, not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
In order to more clearly illustrate the method provided by the present invention, the following examples are used to describe the methods for testing the indexes of the flame retardant carpet fabric prepared in the examples and comparative examples as follows:
flame retardancy: the flame retardant carpet face fabric prepared by the same size of examples and comparative examples was tested with reference to GB/T5454-test limiting oxygen index.
Mechanical properties: the flame retardant carpets prepared in the same size examples and comparative examples were tested for breaking strength with reference to GB/T3923.1.
Example 1
(1) Uniformly mixing and stirring siloxane monomers, methanol and tetrahydrofuran according to a mass ratio of 1:5:15, heating to 52 ℃, preserving heat for 10min, dropwise adding hydrochloric acid with a mass fraction of 0.5% of siloxane monomer 2 at a rate of 3ml/min, continuously reacting for 4h, adjusting pH to 6.8 by using sodium bicarbonate, and performing rotary evaporation at 55 ℃ to obtain hyperbranched polysiloxane; mixing hyperbranched polysiloxane and deionized water according to a mass ratio of 1:1.3, uniformly stirring, regulating pH to 5 by using hydrochloric acid, heating to 50 ℃, reacting for 4 hours, performing rotary evaporation, and vacuum drying at 55 ℃ to obtain amino-terminated hyperbranched polysiloxane;
(2) Mixing stearic acid and diethylenetriamine according to a mass ratio of 1:1, heating to 150 ℃, controlling the reaction pressure to 8kPa, continuously heating to 190 ℃ after reacting for 3 hours, controlling the pressure to 5.05kPa, transferring to a nitrogen atmosphere, continuously reacting for 3 hours, dropwise adding benzyl chloride with the mass of 0.2 times of that of stearic acid at a rate of 1ml/min, transferring to an oil bath, reacting at 105 ℃ for 2 hours while preserving heat, cooling to room temperature, adding thiourea with the mass of 1.1 times of that of stearic acid, and continuously reacting for 1 hour to obtain thioureido imidazoline quaternary ammonium salt; mixing thiouroyl imidazoline quaternary ammonium salt and ethanol according to the mass ratio of 1:25, stirring until the mixture is dissolved, adding copper acetate-hydrate with the mass of 0.4 times of the thiouroyl imidazoline quaternary ammonium salt, stirring at 100rpm for reaction for 20min, heating to 110 ℃, carrying out reflux reaction for 24h, filtering, washing with absolute ethanol and deionized water for 3 times, and drying until the weight is constant to obtain the thiouroyl imidazoline quaternary ammonium copper complex;
(3) Mixing amino-terminated hyperbranched polysiloxane and thiourea-based imidazoline quaternary ammonium copper complex in a mass ratio of 50:1-80:3, and placing in an internal mixer for banburying for 5 hours to prepare a self-made flame retardant;
(4) Placing polyurethane into a reaction kettle, preheating for 5-min at 70 ℃, sequentially adding self-made flame retardant, hydrogen-containing silicone oil, lignocellulose, defoamer polydimethylsiloxane and ethanol, wherein the mass ratio of the polyurethane to the self-made flame retardant to the hydrogen-containing silicone oil to the lignocellulose to the defoamer to the ethanol is 7:1:0.5:1:0.002:2, heating to 100 ℃, preserving heat for 30min, and transferring to a loom to obtain polyurethane base cloth;
(5) Mixing aniline and hydrochloric acid with the mass fraction of 2% according to the mass ratio of 1:8, uniformly stirring to prepare an aniline solution, immersing polyacrylonitrile fibers in the aniline solution, stirring at 100rpm, dropwise adding ammonium persulfate serving as an initiator with the mass of 0.03 times of that of the aniline at the rate of 1ml/min, continuously stirring and reacting until the color is changed into dark green, continuously reacting for 2 hours, and fishing out for alkali treatment and ionic liquid post-treatment, wherein the alkali treatment comprises the following steps: immersing in a sodium hydroxide solution with the mass fraction of 4%, heating to 70 ℃, treating for 20min, and washing with deionized water for 2min; the post-treatment process of the ionic liquid comprises the following steps: mixing cotton fiber and ionic liquid chloridized 1-butyl-3-methylimidazole according to a mass ratio of 1:10, heating to 90 ℃, stirring at 100rpm for reaction for 5 hours, filtering, immersing the polyacrylonitrile fiber subjected to alkali treatment, and standing for 8 hours; preparing modified polyacrylonitrile fibers; after double twisting, spinning and weaving, the yarn with the gram weight of 200g/m is prepared 2 Acrylic base cloth;
(6) And arranging the polyurethane base cloth and the acrylic fiber base in a pressing machine, and pressing for 2min at 110 ℃ to obtain the flame-retardant carpet fabric.
Example 2
(1) Uniformly mixing and stirring siloxane monomers, methanol and tetrahydrofuran according to a mass ratio of 1:5:18, heating to 54 ℃, preserving heat for 15min, dropwise adding hydrochloric acid with a mass fraction of 0.8% of the siloxane monomers 3 at a rate of 4ml/min, continuously reacting for 5h, adjusting pH to 7.0 by using sodium bicarbonate, and performing rotary evaporation at a temperature of 60 ℃ to obtain hyperbranched polysiloxane; mixing hyperbranched polysiloxane and deionized water according to a mass ratio of 1:1.5, uniformly stirring, regulating pH to 5 by using hydrochloric acid, heating to 53 ℃, reacting for 5 hours, performing rotary evaporation, and vacuum drying at 60 ℃ to obtain amino-terminated hyperbranched polysiloxane;
(2) Mixing stearic acid and diethylenetriamine according to a mass ratio of 1:1.1, heating to 155 ℃, controlling the reaction pressure to 8.15kPa, continuously heating to 195 ℃ after reacting for 4 hours, controlling the pressure to 5.06kPa, transferring to a nitrogen atmosphere, continuously reacting for 4 hours, dropwise adding benzyl chloride with the mass of 0.3 times of that of stearic acid at a rate of 1ml/min, transferring to an oil bath, reacting for 2.5 hours at a temperature of 105-115 ℃, cooling to room temperature, adding thiourea with the mass of 1.2 times of that of stearic acid, and continuously reacting for 1.5 hours to obtain thioureido imidazoline quaternary ammonium salt; mixing thiouroyl imidazoline quaternary ammonium salt and ethanol according to the mass ratio of 1:20, stirring until the mixture is dissolved, adding copper acetate-hydrate with the mass of 0.5 times of the thiouroyl imidazoline quaternary ammonium salt, stirring at 150rpm for reaction for 30min, heating to 115 ℃, carrying out reflux reaction for 24h, filtering, washing with absolute ethanol and deionized water for 4 times, and drying until the weight is constant to obtain the thiouroyl imidazoline quaternary ammonium copper complex;
(3) Mixing amino-terminated hyperbranched polysiloxane and thiourea-based imidazoline quaternary ammonium copper complex according to the mass ratio of 65:2, placing the mixture into an internal mixer, and banburying for 6 hours to prepare a self-made flame retardant;
(4) Placing polyurethane into a reaction kettle, preheating for 6min at 75 ℃, sequentially adding a self-made flame retardant, hydrogen-containing silicone oil, lignocellulose, a defoaming agent polyoxyethylene polyoxypropylene pentaerythritol ether and ethanol, wherein the mass ratio of the polyurethane to the self-made flame retardant to the hydrogen-containing silicone oil to the lignocellulose to the defoaming agent to the ethanol is 8:1.2:0.6:1.5:0.007:2.5, heating to 110 ℃, preserving heat for 40min, and transferring to a loom to obtain polyurethane base cloth;
(5) Mixing aniline and hydrochloric acid with the mass fraction of 3% according to the mass ratio of 1:9, uniformly stirring to obtain an aniline solution, immersing polyacrylonitrile fibers in the aniline solution, stirring at 150rpm, dropwise adding ammonium persulfate serving as an initiator with the mass of 0.05 times of that of the aniline at the speed of 1ml/min, continuously stirring and reacting until the color is changed into dark green, continuously reacting for 2.5h, and fishing out for alkali treatment and ionic liquid post-treatment, wherein the alkali treatment comprises the following steps: immersing in 5% sodium hydroxide solution, heating to 75deg.C, treating for 25min,washing with deionized water for 2.5min; the post-treatment process of the ionic liquid comprises the following steps: mixing cotton fiber and ionic liquid chloridized 1-butyl-3-methylimidazole according to a mass ratio of 1:15, heating to 100 ℃, stirring at 150rpm for reaction for 5.5 hours, filtering, immersing the polyacrylonitrile fiber subjected to alkali treatment, and standing for 10 hours; preparing modified polyacrylonitrile fibers; after double twisting, spinning and weaving, the yarn with the gram weight of 300g/m is prepared 2 Acrylic base cloth;
(6) And arranging the polyurethane base cloth and the acrylic fiber base in a pressing machine, and pressing for 3min at 115 ℃ to obtain the flame-retardant carpet fabric.
Example 3
(1) Uniformly mixing and stirring siloxane monomers, methanol and tetrahydrofuran according to a mass ratio of 1:5:20, heating to 55 ℃, preserving heat for 20min, dropwise adding hydrochloric acid with a mass fraction of 1.5% of siloxane monomers 4 at a rate of 5ml/min, continuously reacting for 6h, adjusting pH to 7.2 by using sodium bicarbonate, and performing rotary evaporation at 65 ℃ to obtain hyperbranched polysiloxane; mixing hyperbranched polysiloxane and deionized water according to a mass ratio of 1:1.6, uniformly stirring, regulating pH to 5 by using hydrochloric acid, heating to 55 ℃, reacting for 6 hours, performing rotary evaporation, and vacuum drying at 65 ℃ to obtain amino-terminated hyperbranched polysiloxane;
(2) Mixing stearic acid and diethylenetriamine according to a mass ratio of 1:1.2, heating to 160 ℃, controlling the reaction pressure to 8.3kPa, reacting for 5 hours, continuously heating to 200 ℃, controlling the pressure to 5.07kPa, transferring to a nitrogen atmosphere, continuously reacting for 5 hours, dropwise adding benzyl chloride with the mass of 0.4 times of that of stearic acid at a rate of 2ml/min, transferring to an oil bath, reacting for 3 hours at 115 ℃ in a heat-preserving manner, cooling to room temperature, adding thiourea with the mass of 1.3 times of that of stearic acid, and continuously reacting for 2 hours to obtain thiourea-based imidazoline quaternary ammonium salt; mixing thiouroyl imidazoline quaternary ammonium salt and ethanol according to the mass ratio of 1:50, stirring until the mixture is dissolved, adding copper acetate-hydrate with the mass of 0.6 times of the thiouroyl imidazoline quaternary ammonium salt, stirring at 200rpm for reaction for 40min, heating to 120 ℃, carrying out reflux reaction for 24h, filtering, washing with absolute ethanol and deionized water for 5 times, and drying until the weight is constant to obtain the thiouroyl imidazoline quaternary ammonium copper complex;
(3) Mixing amino-terminated hyperbranched polysiloxane and thiourea-based imidazoline quaternary ammonium copper complex in a mass ratio of 50:1-80:3, and placing in an internal mixer for banburying for 8 hours to prepare a self-made flame retardant;
(4) Placing polyurethane into a reaction kettle, preheating for 8min at 80 ℃, sequentially adding a self-made flame retardant, hydrogen-containing silicone oil, lignocellulose, a defoaming agent polyoxyethylene polyoxypropylene amine ether and ethanol, wherein the mass ratio of the polyurethane to the self-made flame retardant to the hydrogen-containing silicone oil to the lignocellulose to the defoaming agent to the ethanol is 9:1.5:0.8:2:0.012:3, heating to 120 ℃, preserving heat for 50min, and transferring to a loom to obtain polyurethane base cloth;
(5) Mixing aniline and hydrochloric acid with the mass fraction of 4% according to the mass ratio of 1:10, uniformly stirring to prepare an aniline solution, immersing polyacrylonitrile fibers in the aniline solution, stirring at 200rpm, dropwise adding ammonium persulfate serving as an initiator with the mass of 0.06 times of that of the aniline at the rate of 2ml/min, continuously stirring and reacting until the color is changed into dark green, continuously reacting for 3 hours, and fishing out for alkali treatment and ionic liquid post-treatment, wherein the alkali treatment comprises the following steps: immersing in 6% sodium hydroxide solution by mass fraction, heating to 80 ℃, treating for 30min, and washing with deionized water for 3min; the post-treatment process of the ionic liquid comprises the following steps: mixing cotton fiber and ionic liquid chloridized 1-butyl-3-methylimidazole according to a mass ratio of 1:20, heating to 110 ℃, stirring at 200rpm for reaction for 6 hours, filtering, immersing the polyacrylonitrile fiber subjected to alkali treatment, and standing for 12 hours; preparing modified polyacrylonitrile fibers; after double twisting, spinning and weaving, the yarn with the gram weight of 400g/m is prepared 2 Acrylic base cloth;
(6) And arranging the polyurethane base cloth and the acrylic fiber base in a pressing machine, and pressing for 4min at 120 ℃ to obtain the flame-retardant carpet fabric.
Comparative example 1
(1) Mixing stearic acid and diethylenetriamine according to a mass ratio of 1:1.1, heating to 155 ℃, controlling the reaction pressure to 8.15kPa, continuously heating to 195 ℃ after reacting for 4 hours, controlling the pressure to 5.06kPa, transferring to a nitrogen atmosphere, continuously reacting for 4 hours, dropwise adding benzyl chloride with the mass of 0.3 times of that of stearic acid at a rate of 1ml/min, transferring to an oil bath, reacting for 2.5 hours at a temperature of 105-115 ℃, cooling to room temperature, adding thiourea with the mass of 1.2 times of that of stearic acid, and continuously reacting for 1.5 hours to obtain thioureido imidazoline quaternary ammonium salt; mixing thiouroyl imidazoline quaternary ammonium salt and ethanol according to the mass ratio of 1:20, stirring until the mixture is dissolved, adding copper acetate-hydrate with the mass of 0.5 times of the thiouroyl imidazoline quaternary ammonium salt, stirring at 150rpm for reaction for 30min, heating to 115 ℃, carrying out reflux reaction for 24h, filtering, washing with absolute ethanol and deionized water for 4 times, and drying until the weight is constant to obtain the thiouroyl imidazoline quaternary ammonium copper complex;
(2) Placing polyurethane in a reaction kettle, preheating for 6min at 75 ℃, sequentially adding thiourea imidazoline quaternary ammonium copper complex, hydrogen-containing silicone oil, lignocellulose, defoamer polyoxyethylene polyoxypropylene pentaerythritol ether and ethanol, wherein the mass ratio of the polyurethane to the thiourea imidazoline quaternary ammonium copper complex to the hydrogen-containing silicone oil to the lignin cellulose to the defoamer to the ethanol is 8:1.2:0.6:1.5:0.007:2.5, heating to 110 ℃, preserving heat for 40min, and transferring to a loom to obtain polyurethane base cloth;
(5) Mixing aniline and hydrochloric acid with the mass fraction of 3% according to the mass ratio of 1:9, uniformly stirring to obtain an aniline solution, immersing polyacrylonitrile fibers in the aniline solution, stirring at 150rpm, dropwise adding ammonium persulfate serving as an initiator with the mass of 0.05 times of that of the aniline at the speed of 1ml/min, continuously stirring and reacting until the color is changed into dark green, continuously reacting for 2.5h, and fishing out for alkali treatment and ionic liquid post-treatment, wherein the alkali treatment comprises the following steps: immersing in 5% sodium hydroxide solution by mass fraction, heating to 75deg.C, treating for 25min, and washing with deionized water for 2.5min; the post-treatment process of the ionic liquid comprises the following steps: mixing cotton fiber and ionic liquid chloridized 1-butyl-3-methylimidazole according to a mass ratio of 1:15, heating to 100 ℃, stirring at 150rpm for reaction for 5.5 hours, filtering, immersing the polyacrylonitrile fiber subjected to alkali treatment, and standing for 10 hours; preparing modified polyacrylonitrile fibers; after double twisting, spinning and weaving, the yarn with the gram weight of 300g/m is prepared 2 Acrylic base cloth;
(6) And arranging the polyurethane base cloth and the acrylic fiber base in a pressing machine, and pressing for 3min at 115 ℃ to obtain the flame-retardant carpet fabric.
Comparative example 2
(1) Uniformly mixing and stirring siloxane monomers, methanol and tetrahydrofuran according to a mass ratio of 1:5:18, heating to 54 ℃, preserving heat for 15min, dropwise adding hydrochloric acid with a mass fraction of 0.8% of the siloxane monomers 3 at a rate of 4ml/min, continuously reacting for 5h, adjusting pH to 7.0 by using sodium bicarbonate, and performing rotary evaporation at a temperature of 60 ℃ to obtain hyperbranched polysiloxane; mixing hyperbranched polysiloxane and deionized water according to a mass ratio of 1:1.5, uniformly stirring, regulating pH to 5 by using hydrochloric acid, heating to 53 ℃, reacting for 5 hours, performing rotary evaporation, and vacuum drying at 60 ℃ to obtain amino-terminated hyperbranched polysiloxane;
(2) Placing polyurethane into a reaction kettle, preheating for 6min at 75 ℃, sequentially adding amino-terminated hyperbranched polysiloxane, hydrogen-containing silicone oil, lignocellulose, defoamer polyoxyethylene polyoxypropylene pentaerythritol ether and ethanol, wherein the mass ratio of the polyurethane to the amino-terminated hyperbranched polysiloxane to the hydrogen-containing silicone oil to the lignin cellulose to the defoamer to the ethanol is 8:1.2:0.6:1.5:0.007:2.5, heating to 110 ℃, preserving heat for 40min, and transferring to a loom to obtain polyurethane base cloth;
(3) Mixing aniline and hydrochloric acid with the mass fraction of 3% according to the mass ratio of 1:9, uniformly stirring to obtain an aniline solution, immersing polyacrylonitrile fibers in the aniline solution, stirring at 150rpm, dropwise adding ammonium persulfate serving as an initiator with the mass of 0.05 times of that of the aniline at the speed of 1ml/min, continuously stirring and reacting until the color is changed into dark green, continuously reacting for 2.5h, and fishing out for alkali treatment and ionic liquid post-treatment, wherein the alkali treatment comprises the following steps: immersing in 5% sodium hydroxide solution by mass fraction, heating to 75deg.C, treating for 25min, and washing with deionized water for 2.5min; the post-treatment process of the ionic liquid comprises the following steps: mixing cotton fiber and ionic liquid chloridized 1-butyl-3-methylimidazole according to a mass ratio of 1:15, heating to 100 ℃, stirring at 150rpm for reaction for 5.5 hours, filtering, immersing the polyacrylonitrile fiber subjected to alkali treatment, and standing for 10 hours; preparing modified polyacrylonitrile fibers; after double twisting, spinning and weaving, the yarn with the gram weight of 300g/m is prepared 2 Acrylic base cloth;
(4) And arranging the polyurethane base cloth and the acrylic fiber base in a pressing machine, and pressing for 3min at 115 ℃ to obtain the flame-retardant carpet fabric.
Comparative example 3
(1) Uniformly mixing and stirring siloxane monomers, methanol and tetrahydrofuran according to a mass ratio of 1:5:18, heating to 54 ℃, preserving heat for 15min, dropwise adding hydrochloric acid with a mass fraction of 0.8% of the siloxane monomers 3 at a rate of 4ml/min, continuously reacting for 5h, adjusting pH to 7.0 by using sodium bicarbonate, and performing rotary evaporation at a temperature of 60 ℃ to obtain hyperbranched polysiloxane; mixing hyperbranched polysiloxane and deionized water according to a mass ratio of 1:1.5, uniformly stirring, regulating pH to 5 by using hydrochloric acid, heating to 53 ℃, reacting for 5 hours, performing rotary evaporation, and vacuum drying at 60 ℃ to obtain amino-terminated hyperbranched polysiloxane;
(2) Mixing stearic acid and diethylenetriamine according to a mass ratio of 1:1.1, heating to 155 ℃, controlling the reaction pressure to 8.15kPa, continuously heating to 195 ℃ after reacting for 4 hours, controlling the pressure to 5.06kPa, transferring to a nitrogen atmosphere, continuously reacting for 4 hours, dropwise adding benzyl chloride with the mass of 0.3 times of that of stearic acid at a rate of 1ml/min, transferring to an oil bath, reacting for 2.5 hours at a temperature of 105-115 ℃, cooling to room temperature, adding thiourea with the mass of 1.2 times of that of stearic acid, and continuously reacting for 1.5 hours to obtain thioureido imidazoline quaternary ammonium salt; mixing thiouroyl imidazoline quaternary ammonium salt and ethanol according to the mass ratio of 1:20, stirring until the mixture is dissolved, adding copper acetate-hydrate with the mass of 0.5 times of the thiouroyl imidazoline quaternary ammonium salt, stirring at 150rpm for reaction for 30min, heating to 115 ℃, carrying out reflux reaction for 24h, filtering, washing with absolute ethanol and deionized water for 4 times, and drying until the weight is constant to obtain the thiouroyl imidazoline quaternary ammonium copper complex;
(3) Mixing amino-terminated hyperbranched polysiloxane and thiourea-based imidazoline quaternary ammonium copper complex according to the mass ratio of 65:2, placing the mixture into an internal mixer, and banburying for 6 hours to prepare a self-made flame retardant;
(4) Placing polyurethane into a reaction kettle, preheating for 6min at 75 ℃, sequentially adding a self-made flame retardant, hydrogen-containing silicone oil, lignocellulose, a defoaming agent polyoxyethylene polyoxypropylene pentaerythritol ether and ethanol, wherein the mass ratio of the polyurethane to the self-made flame retardant to the hydrogen-containing silicone oil to the lignocellulose to the defoaming agent to the ethanol is 8:1.2:0.6:1.5:0.007:2.5, heating to 110 ℃, preserving heat for 40min, and transferring to a loom to obtain polyurethane base cloth;
(5) The polyacrylonitrile fiber is subjected to double twisting, spinning and weaving to obtain the polyacrylonitrile fiber with the gram weight of 300g/m 2 Acrylic base cloth;
(6) And arranging the polyurethane base cloth and the acrylic fiber base in a pressing machine, and pressing for 3min at 115 ℃ to obtain the flame-retardant carpet fabric.
Comparative example 4
(1) Uniformly mixing and stirring siloxane monomers, methanol and tetrahydrofuran according to a mass ratio of 1:5:18, heating to 54 ℃, preserving heat for 15min, dropwise adding hydrochloric acid with a mass fraction of 0.8% of the siloxane monomers 3 at a rate of 4ml/min, continuously reacting for 5h, adjusting pH to 7.0 by using sodium bicarbonate, and performing rotary evaporation at a temperature of 60 ℃ to obtain hyperbranched polysiloxane; mixing hyperbranched polysiloxane and deionized water according to a mass ratio of 1:1.5, uniformly stirring, regulating pH to 5 by using hydrochloric acid, heating to 53 ℃, reacting for 5 hours, performing rotary evaporation, and vacuum drying at 60 ℃ to obtain amino-terminated hyperbranched polysiloxane;
(2) Mixing stearic acid and diethylenetriamine according to a mass ratio of 1:1.1, heating to 155 ℃, controlling the reaction pressure to 8.15kPa, continuously heating to 195 ℃ after reacting for 4 hours, controlling the pressure to 5.06kPa, transferring to a nitrogen atmosphere, continuously reacting for 4 hours, dropwise adding benzyl chloride with the mass of 0.3 times of that of stearic acid at a rate of 1ml/min, transferring to an oil bath, reacting for 2.5 hours at a temperature of 105-115 ℃, cooling to room temperature, adding thiourea with the mass of 1.2 times of that of stearic acid, and continuously reacting for 1.5 hours to obtain thioureido imidazoline quaternary ammonium salt; mixing thiouroyl imidazoline quaternary ammonium salt and ethanol according to the mass ratio of 1:20, stirring until the mixture is dissolved, adding copper acetate-hydrate with the mass of 0.5 times of the thiouroyl imidazoline quaternary ammonium salt, stirring at 150rpm for reaction for 30min, heating to 115 ℃, carrying out reflux reaction for 24h, filtering, washing with absolute ethanol and deionized water for 4 times, and drying until the weight is constant to obtain the thiouroyl imidazoline quaternary ammonium copper complex;
(3) Mixing amino-terminated hyperbranched polysiloxane and thiourea-based imidazoline quaternary ammonium copper complex according to the mass ratio of 65:2, placing the mixture into an internal mixer, and banburying for 6 hours to prepare a self-made flame retardant;
(4) Placing polyurethane into a reaction kettle, preheating for 6min at 75 ℃, sequentially adding a self-made flame retardant, hydrogen-containing silicone oil, lignocellulose, a defoaming agent polyoxyethylene polyoxypropylene pentaerythritol ether and ethanol, wherein the mass ratio of the polyurethane to the self-made flame retardant to the hydrogen-containing silicone oil to the lignocellulose to the defoaming agent to the ethanol is 8:1.2:0.6:1.5:0.007:2.5, heating to 110 ℃, preserving heat for 40min, and transferring to a loom to obtain the polyurethane base fabric, namely the flame-retardant carpet fabric.
Effect example
The following table 1 gives the results of performance analysis of the flame retardant carpet face materials employing examples 1 to 3 of the present invention and comparative examples 1 to 4:
TABLE 1
As is evident from comparison of the experimental data of examples and comparative examples in Table 1, the mechanical strength and flame retardance of the flame retardant carpet face fabric prepared in examples 1, 2 and 3 are better.
It will be evident to those skilled in the art that the invention is not limited to the details of the foregoing illustrative embodiments, and that the present invention may be embodied in other specific forms without departing from the spirit or essential characteristics thereof. The present embodiments are, therefore, to be considered in all respects as illustrative and not restrictive, the scope of the invention being indicated by the appended claims rather than by the foregoing description, and all changes which come within the meaning and range of equivalency of the claims are therefore intended to be embraced therein. Any reference sign in a claim should not be construed as limiting the claim concerned.
Claims (10)
1. The fabric for the flame-retardant carpet is characterized in that the fabric for the flame-retardant carpet is prepared by laminating polyurethane base cloth and acrylic base cloth; the polyurethane base cloth comprises polyurethane, self-made flame retardant, hydrogen-containing silicone oil, lignocellulose, defoamer and ethanol; the acrylic base cloth is woven by modified polyacrylonitrile fibers; the defoaming agent is one or more of polydimethylsiloxane, polyoxyethylene polyoxypropylene pentaerythritol ether and polyoxyethylene polyoxypropylene alcohol amine ether.
2. The fabric for the flame-retardant carpet of claim 1, wherein the self-made flame retardant is prepared by reacting thiourea-based imidazoline quaternary ammonium copper complex with amino-terminated hyperbranched polysiloxane; the thioureido imidazoline quaternary ammonium copper complex is prepared by reacting thioureido imidazoline quaternary ammonium salt with copper acetate-hydrate.
3. The flame-retardant carpet fabric according to claim 2, wherein the thioureido imidazoline quaternary ammonium salt is prepared by using stearic acid and diethylenetriamine as reaction raw materials, performing amidation reaction and cyclization reaction, performing quaternization reaction with benzyl chloride, and finally introducing thiourea.
4. The flame-retardant carpet fabric according to claim 1, wherein the modified polyacrylonitrile fiber is prepared by polymerizing aniline on the surface of the polyacrylonitrile fiber, then performing alkali treatment, and then performing post-treatment with an ionic liquid with cellulose.
5. The preparation method of the fabric for the flame-retardant carpet is characterized by comprising the following specific steps of:
(1) Mixing hyperbranched polysiloxane and deionized water according to a mass ratio of 1:1.3-1:1.6, uniformly stirring, regulating pH to 5 by hydrochloric acid, heating to 50-55 ℃, reacting for 4-6 hours, performing rotary evaporation, and vacuum drying at 55-65 ℃ to obtain amino-terminated hyperbranched polysiloxane;
(2) Mixing thioureido imidazoline quaternary ammonium salt and ethanol according to the mass ratio of 1:25-1:50, stirring until the mixture is dissolved, adding copper acetate-hydrate with the mass of 0.4-0.6 times that of the thioureido imidazoline quaternary ammonium salt, stirring at 100-200 rpm for reaction for 20-40 min, heating to 110-120 ℃, carrying out reflux reaction for 24h, filtering, washing with absolute ethanol and deionized water for 3-5 times, and drying until the weight is constant, thus obtaining the thioureido imidazoline quaternary ammonium copper complex;
(3) Mixing the amino-terminated hyperbranched polysiloxane and the thiourea-based imidazoline quaternary ammonium copper complex in a mass ratio of 50:1-80:3, and placing the mixture in an internal mixer for banburying for 5-8 hours to prepare a self-made flame retardant;
(4) Placing polyurethane into a reaction kettle, preheating for 5-8 min at 70-80 ℃, sequentially adding a self-made flame retardant, hydrogen-containing silicone oil, lignocellulose, a defoaming agent and ethanol, heating to 100-120 ℃, preserving heat for 30-50 min, and transferring to a loom to obtain polyurethane base cloth;
(5) Mixing aniline and hydrochloric acid with the mass fraction of 2-4% according to the mass ratio of 1:8-1:10, uniformly stirring to obtain an aniline solution, immersing polyacrylonitrile fibers in the aniline solution, stirring at 100-200 rpm, dropwise adding ammonium persulfate serving as an initiator with the mass of 0.03-0.06 times of that of the aniline at the speed of 1-2 ml/min, continuously stirring to react until the color is changed into dark green, continuously reacting for 2-3 h, and fishing out to perform alkali treatment and ionic liquid aftertreatment to obtain modified polyacrylonitrile fibers; after double twisting, spinning and weaving, the yarn with the gram weight of 200 to 400g/m is prepared 2 Acrylic base cloth;
(6) Arranging the polyurethane base cloth and the acrylic fiber base in a pressing machine, and pressing for 2-4 min at 110-120 ℃ to obtain the flame-retardant carpet fabric.
6. The method of producing a flame retardant carpet tile according to claim 5, wherein in step (1): the preparation method of the hyperbranched polysiloxane comprises the following steps: uniformly mixing and stirring siloxane monomers, methanol and tetrahydrofuran according to the mass ratio of 1:5:15-1:5:20, heating to 52-55 ℃, preserving heat for 10-20 min, dropwise adding hydrochloric acid with the mass fraction of 0.5-1.5% of the siloxane monomers at the rate of 3-5 ml/min into the mixture, continuously reacting for 4-6 h, adjusting the pH to 6.8-7.2 by using sodium bicarbonate, and performing rotary evaporation at the temperature of 55-65 ℃ to obtain the hyperbranched polysiloxane.
7. The method of producing a flame retardant carpet tile according to claim 5, wherein in step (2): the preparation method of the thioureido imidazoline quaternary ammonium salt comprises the following steps: mixing stearic acid and diethylenetriamine according to a mass ratio of 1:1-1:1.2, heating to 150-160 ℃, controlling the reaction pressure to 8-8.3 kPa, reacting for 3-5 hours, continuously heating to 190-200 ℃, controlling the pressure to 5.05-5.07 kPa, transferring to a nitrogen atmosphere, continuously reacting for 3-5 hours, dropwise adding benzyl chloride with a mass of 0.2-0.4 times of stearic acid at a speed of 1-2 ml/min, transferring to an oil bath, reacting for 2-3 hours at a temperature of 105-115 ℃, cooling to room temperature, adding thiourea with a mass of 1.1-1.3 times of stearic acid, and continuously reacting for 1-2 hours to obtain the thioureido imidazoline quaternary ammonium salt.
8. The method of producing a flame retardant carpet tile according to claim 5, wherein in step (4): the mass ratio of the polyurethane to the self-made flame retardant to the hydrogen-containing silicone oil to the lignocellulose to the defoamer to the ethanol is 7:1:0.5:1:0.002:2-9:1.5:0.8:2:0.012:3.
9. The method of producing a flame retardant carpet tile according to claim 5, wherein in step (5): the alkali treatment process comprises the following steps: immersing in sodium hydroxide solution with the mass fraction of 4-6%, heating to 70-80 ℃, treating for 20-30 min, and washing with deionized water for 2-3 min.
10. The method of producing a flame retardant carpet tile according to claim 5, wherein in step (5): the post-treatment process of the ionic liquid comprises the following steps: mixing cotton fiber and ionic liquid chloridized 1-butyl-3-methylimidazole according to a mass ratio of 1:10-1:20, heating to 90-110 ℃, stirring at 100-200 rpm for reaction for 5-6 hours, filtering, immersing the polyacrylonitrile fiber subjected to alkali treatment, and standing for 8-12 hours.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202310222881.0A CN117863699A (en) | 2023-03-09 | 2023-03-09 | Flame-retardant carpet fabric and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202310222881.0A CN117863699A (en) | 2023-03-09 | 2023-03-09 | Flame-retardant carpet fabric and preparation method thereof |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN117863699A true CN117863699A (en) | 2024-04-12 |
Family
ID=90587108
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202310222881.0A Pending CN117863699A (en) | 2023-03-09 | 2023-03-09 | Flame-retardant carpet fabric and preparation method thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN117863699A (en) |
-
2023
- 2023-03-09 CN CN202310222881.0A patent/CN117863699A/en active Pending
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| EP3257975A1 (en) | Acetic nitrile fibre and preparation method therefor | |
| CN110627965B (en) | Photochromic waterborne polyurethane coating agent and preparation method thereof | |
| CN106750324B (en) | Polyquaternary amino polyether polydimethylsiloxane, preparation method thereof and hand feeling finishing agent | |
| CN112442894A (en) | Preparation method of durable flame-retardant silk product | |
| CN111485427A (en) | Method capable of enhancing hydrophilic property of cotton fiber | |
| CN117863699A (en) | Flame-retardant carpet fabric and preparation method thereof | |
| CN116288812B (en) | Preparation method and application of bio-based spandex fiber fabric | |
| CN110130104A (en) | A kind of Flame Retarded Silk Fibers fabric and preparation method thereof based on biomass | |
| CN110172751A (en) | A kind of carbon fibre and its carbonization method | |
| CN113564924A (en) | Finishing method for realizing self-adjustment of air permeability of polyester fabric | |
| CN116427173A (en) | Washable flame-retardant anti-dripping polyester cotton 65/35 fabric and preparation method thereof | |
| CN116463844A (en) | Crease-resistant casual suit fabric and production process thereof | |
| CN109267355A (en) | A kind of preparation method of silicone oil softener | |
| CN113291039B (en) | Processing method of flame-retardant waterproof moisture-permeable composite fabric | |
| CN113005781B (en) | Conductive fabric processing method based on cascade catalytic graft polymerization | |
| CN114381932A (en) | Light anti-static fabric and preparation method thereof | |
| CN113463264A (en) | Preparation method of warp-knitted fabric with moisture absorption and quick-drying cool feeling functions and product thereof | |
| CN112609464A (en) | Dyeing process of hydrophobic imine fiber textile | |
| CN117265694B (en) | Method for preparing bio-based PTT fiber by recycling waste fabric | |
| CN116334784B (en) | Waterproof functional fiber material and preparation method and application thereof | |
| CN110105577B (en) | Preparation method of reactive silicon-phosphorus-nitrogen synergistic flame-retardant water-repellent functional auxiliary for cotton | |
| CN117447723B (en) | Preparation method of organic silicon emulsion | |
| CN110592946B (en) | Flame-retardant finishing method for polyacrylonitrile carbon fibers | |
| CN116770580A (en) | Manufacturing method of post-treatment modified flame-retardant fiber | |
| CN115305722B (en) | Photochromic fabric and preparation method thereof |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination |