CN111041816B - Preparation of flame-retardant smoke-inhibiting PVC film - Google Patents
Preparation of flame-retardant smoke-inhibiting PVC film Download PDFInfo
- Publication number
- CN111041816B CN111041816B CN201911248029.0A CN201911248029A CN111041816B CN 111041816 B CN111041816 B CN 111041816B CN 201911248029 A CN201911248029 A CN 201911248029A CN 111041816 B CN111041816 B CN 111041816B
- Authority
- CN
- China
- Prior art keywords
- flame
- pvc film
- retardant
- temperature
- polyoxometallate
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
- 239000003063 flame retardant Substances 0.000 title claims abstract description 54
- 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 53
- 239000000779 smoke Substances 0.000 title claims abstract description 13
- 238000002360 preparation method Methods 0.000 title claims abstract description 12
- 230000002401 inhibitory effect Effects 0.000 title description 2
- 238000009987 spinning Methods 0.000 claims abstract description 23
- 239000002243 precursor Substances 0.000 claims abstract description 21
- 238000010041 electrostatic spinning Methods 0.000 claims abstract description 19
- 238000001035 drying Methods 0.000 claims abstract description 15
- 230000000694 effects Effects 0.000 claims abstract description 12
- 230000002195 synergetic effect Effects 0.000 claims abstract description 12
- 238000003756 stirring Methods 0.000 claims abstract description 8
- 238000002791 soaking Methods 0.000 claims abstract description 7
- BHTBHKFULNTCHQ-UHFFFAOYSA-H zinc;tin(4+);hexahydroxide Chemical group [OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[Zn+2].[Sn+4] BHTBHKFULNTCHQ-UHFFFAOYSA-H 0.000 claims description 8
- 229910052782 aluminium Inorganic materials 0.000 claims description 5
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical group [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 5
- 239000011888 foil Substances 0.000 claims description 5
- 229910052751 metal Inorganic materials 0.000 claims description 5
- 239000002184 metal Substances 0.000 claims description 5
- 238000000034 method Methods 0.000 claims 1
- 239000012796 inorganic flame retardant Substances 0.000 abstract description 6
- 231100000956 nontoxicity Toxicity 0.000 abstract description 4
- 230000001629 suppression Effects 0.000 abstract description 4
- 229920000915 polyvinyl chloride Polymers 0.000 description 54
- 239000004800 polyvinyl chloride Substances 0.000 description 54
- 239000000243 solution Substances 0.000 description 34
- 239000003795 chemical substances by application Substances 0.000 description 12
- ADCOVFLJGNWWNZ-UHFFFAOYSA-N antimony trioxide Chemical compound O=[Sb]O[Sb]=O ADCOVFLJGNWWNZ-UHFFFAOYSA-N 0.000 description 6
- 238000001907 polarising light microscopy Methods 0.000 description 5
- 229920006324 polyoxymethylene Polymers 0.000 description 5
- 125000000962 organic group Chemical group 0.000 description 4
- -1 polyethylene Polymers 0.000 description 4
- 239000000463 material Substances 0.000 description 3
- 239000004698 Polyethylene Substances 0.000 description 2
- 239000004743 Polypropylene Substances 0.000 description 2
- 239000007864 aqueous solution Substances 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 230000003197 catalytic effect Effects 0.000 description 2
- 238000002485 combustion reaction Methods 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 239000011159 matrix material Substances 0.000 description 2
- 230000010412 perfusion Effects 0.000 description 2
- 229920000573 polyethylene Polymers 0.000 description 2
- 239000002861 polymer material Substances 0.000 description 2
- 229920001155 polypropylene Polymers 0.000 description 2
- 239000011829 room temperature ionic liquid solvent Substances 0.000 description 2
- MQIUGAXCHLFZKX-UHFFFAOYSA-N Di-n-octyl phthalate Natural products CCCCCCCCOC(=O)C1=CC=CC=C1C(=O)OCCCCCCCC MQIUGAXCHLFZKX-UHFFFAOYSA-N 0.000 description 1
- 239000002841 Lewis acid Substances 0.000 description 1
- 239000004793 Polystyrene Substances 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000004075 alteration Effects 0.000 description 1
- 238000005452 bending Methods 0.000 description 1
- BJQHLKABXJIVAM-UHFFFAOYSA-N bis(2-ethylhexyl) phthalate Chemical compound CCCCC(CC)COC(=O)C1=CC=CC=C1C(=O)OCC(CC)CCCC BJQHLKABXJIVAM-UHFFFAOYSA-N 0.000 description 1
- 230000000711 cancerogenic effect Effects 0.000 description 1
- 231100000315 carcinogenic Toxicity 0.000 description 1
- 229910052801 chlorine Inorganic materials 0.000 description 1
- 125000001309 chloro group Chemical group Cl* 0.000 description 1
- 238000007598 dipping method Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000011049 filling Methods 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 229910052736 halogen Inorganic materials 0.000 description 1
- 150000002367 halogens Chemical class 0.000 description 1
- 125000004435 hydrogen atom Chemical group [H]* 0.000 description 1
- 150000007517 lewis acids Chemical class 0.000 description 1
- 229920001684 low density polyethylene Polymers 0.000 description 1
- 239000004702 low-density polyethylene Substances 0.000 description 1
- 229910044991 metal oxide Inorganic materials 0.000 description 1
- 150000004706 metal oxides Chemical class 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- MEFBJEMVZONFCJ-UHFFFAOYSA-N molybdate Chemical compound [O-][Mo]([O-])(=O)=O MEFBJEMVZONFCJ-UHFFFAOYSA-N 0.000 description 1
- 239000004014 plasticizer Substances 0.000 description 1
- 229920002223 polystyrene Polymers 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 239000012747 synergistic agent Substances 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
- 230000002087 whitening effect Effects 0.000 description 1
Classifications
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M11/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising
- D06M11/32—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with oxygen, ozone, ozonides, oxides, hydroxides or percompounds; Salts derived from anions with an amphoteric element-oxygen bond
- D06M11/36—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with oxygen, ozone, ozonides, oxides, hydroxides or percompounds; Salts derived from anions with an amphoteric element-oxygen bond with oxides, hydroxides or mixed oxides; with salts derived from anions with an amphoteric element-oxygen bond
- D06M11/48—Oxides or hydroxides of chromium, molybdenum or tungsten; Chromates; Dichromates; Molybdates; Tungstates
-
- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
- D01D5/00—Formation of filaments, threads, or the like
- D01D5/0007—Electro-spinning
- D01D5/0015—Electro-spinning characterised by the initial state of the material
- D01D5/003—Electro-spinning characterised by the initial state of the material the material being a polymer solution or dispersion
-
- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
- D01D5/00—Formation of filaments, threads, or the like
- D01D5/0007—Electro-spinning
- D01D5/0061—Electro-spinning characterised by the electro-spinning apparatus
-
- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
- D01D5/00—Formation of filaments, threads, or the like
- D01D5/0007—Electro-spinning
- D01D5/0061—Electro-spinning characterised by the electro-spinning apparatus
- D01D5/0076—Electro-spinning characterised by the electro-spinning apparatus characterised by the collecting device, e.g. drum, wheel, endless belt, plate or grid
-
- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
- D01D5/00—Formation of filaments, threads, or the like
- D01D5/0007—Electro-spinning
- D01D5/0061—Electro-spinning characterised by the electro-spinning apparatus
- D01D5/0092—Electro-spinning characterised by the electro-spinning apparatus characterised by the electrical field, e.g. combined with a magnetic fields, using biased or alternating fields
-
- 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
- D01F6/00—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof
- D01F6/44—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from mixtures of polymers obtained by reactions only involving carbon-to-carbon unsaturated bonds as major constituent with other polymers or low-molecular-weight compounds
- D01F6/48—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from mixtures of polymers obtained by reactions only involving carbon-to-carbon unsaturated bonds as major constituent with other polymers or low-molecular-weight compounds of polymers of halogenated hydrocarbons
-
- D—TEXTILES; PAPER
- D04—BRAIDING; LACE-MAKING; KNITTING; TRIMMINGS; NON-WOVEN FABRICS
- D04H—MAKING TEXTILE FABRICS, e.g. FROM FIBRES OR FILAMENTARY MATERIAL; FABRICS MADE BY SUCH PROCESSES OR APPARATUS, e.g. FELTS, NON-WOVEN FABRICS; COTTON-WOOL; WADDING ; NON-WOVEN FABRICS FROM STAPLE FIBRES, FILAMENTS OR YARNS, BONDED WITH AT LEAST ONE WEB-LIKE MATERIAL DURING THEIR CONSOLIDATION
- D04H1/00—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres
- D04H1/40—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres without existing or potential cohesive properties
- D04H1/42—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres without existing or potential cohesive properties characterised by the use of certain kinds of fibres insofar as this use has no preponderant influence on the consolidation of the fleece
- D04H1/4282—Addition polymers
-
- D—TEXTILES; PAPER
- D04—BRAIDING; LACE-MAKING; KNITTING; TRIMMINGS; NON-WOVEN FABRICS
- D04H—MAKING TEXTILE FABRICS, e.g. FROM FIBRES OR FILAMENTARY MATERIAL; FABRICS MADE BY SUCH PROCESSES OR APPARATUS, e.g. FELTS, NON-WOVEN FABRICS; COTTON-WOOL; WADDING ; NON-WOVEN FABRICS FROM STAPLE FIBRES, FILAMENTS OR YARNS, BONDED WITH AT LEAST ONE WEB-LIKE MATERIAL DURING THEIR CONSOLIDATION
- D04H1/00—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres
- D04H1/70—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres characterised by the method of forming fleeces or layers, e.g. reorientation of fibres
- D04H1/72—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres characterised by the method of forming fleeces or layers, e.g. reorientation of fibres the fibres being randomly arranged
- D04H1/728—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres characterised by the method of forming fleeces or layers, e.g. reorientation of fibres the fibres being randomly arranged by electro-spinning
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M2101/00—Chemical constitution of the fibres, threads, yarns, fabrics or fibrous goods made from such materials, to be treated
- D06M2101/16—Synthetic fibres, other than mineral fibres
- D06M2101/18—Synthetic fibres consisting of macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
- D06M2101/22—Polymers or copolymers of halogenated mono-olefins
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M2200/00—Functionality of the treatment composition and/or properties imparted to the textile material
- D06M2200/30—Flame or heat resistance, fire retardancy properties
Landscapes
- Engineering & Computer Science (AREA)
- Textile Engineering (AREA)
- Mechanical Engineering (AREA)
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Manufacturing & Machinery (AREA)
- Dispersion Chemistry (AREA)
- Compositions Of Macromolecular Compounds (AREA)
- Artificial Filaments (AREA)
- Manufacture Of Macromolecular Shaped Articles (AREA)
Abstract
The invention discloses a preparation method of a flame-retardant smoke-suppressing PVC film, which comprises the following steps: A. preparing a precursor solution; B. b, violently stirring the precursor solution prepared in the step A at room temperature to obtain a spinning solution; C. b, performing electrostatic spinning on the spinning solution in the step B to obtain a PVC film, and applying a constant-temperature thermal field in a spinning interval and controlling the temperature of a receiving device during the electrostatic spinning; D. c, drying the PVC film obtained in the step C at room temperature, and E, soaking the PVC film obtained in the step 4 in polyoxometallate solution with the synergistic flame-retardant effect for 10-60min; F. and D, drying the POM modified PVC film obtained in the step E in a vacuum furnace, wherein the inorganic flame retardant used for preparing the flame-retardant smoke-suppressing PVC film has the advantages of high safety, smoke suppression, no toxicity, low price and the like, has stable performance and is not easy to volatilize, meets the energy-saving and environment-friendly idea advocated by the nation, and is matched with polyoxometallate for synergistic flame retardation, so that the flame-retardant smoke-suppressing effect is more obvious.
Description
Technical Field
The invention relates to the technical field of manufacturing of flame-retardant and smoke-suppressing PVC films by doping a novel inorganic smoke-eliminating flame retardant in a PVC spinning solution to prepare a PVC film and dipping a Polyoxometallate (POM) solution, in particular to the preparation of the flame-retardant and smoke-suppressing PVC film.
Background
In recent years, serious fires occur in China, which causes great property loss and casualties, and the main reason for causing the fires is that combustible high polymer materials are used in a large amount in buildings, so that the fire-retardant material has important significance for the flame-retardant research of the high polymer materials. PVC is one of main high molecular materials, although the PVC has better flame retardant property, the PVC has large smoke generation amount during combustion, and a large amount of plasticizer dioctyl phthalate is added in the production process of semi-hard products and soft products, so that the combustion property of the PVC is enhanced, and the flame retardant requirement cannot be met. At present, the inorganic flame retardant mainly used in PVC is antimony trioxide, although the antimony trioxide can play a good flame retardant effect, the smoke generation amount is very large, and the smoke is probably carcinogenic, so that a novel inorganic flame retardant is inevitably found to replace the antimony trioxide.
The PVC mainly contains polyvinyl chloride, is yellowish, semitransparent and glossy. The transparency is better than that of polyethylene and polypropylene, is inferior to that of polystyrene, is divided into soft and hard polyvinyl chloride according to different using amounts of the additives, soft products are soft and tough, the hand feeling is sticky, the hardness of hard products is higher than that of low-density polyethylene and lower than that of polypropylene, and the whitening phenomenon can occur at the bending part. Common preparations: plate, pipe, sole, toy, door and window, wire sheath, stationery, etc. Is a high molecular material which uses a chlorine atom to replace one hydrogen atom in polyethylene.
Polyoxometallate (POMs) is a Lewis acid, has strong acidity and oxidability, and is a green environment-friendly catalytic/synergistic agent with strong adjustability, good thermal stability and good catalytic performance. When the POMs are combined with macromolecular organic groups, the organic-inorganic hybrid room-temperature ionic liquid can be generated, and meanwhile, the POMs have the advantages of the organic group and the macromolecular organic group, have good synergy and simultaneously improve the compatibility of the POMs in a matrix.
Disclosure of Invention
The invention aims to provide a flame-retardant smoke-suppressing PVC film to solve the problems in the background technology.
In order to achieve the purpose, the invention provides the following technical scheme: the preparation method of the flame-retardant smoke-suppressing PVC film comprises the following steps:
A. preparing a precursor solution;
B. b, violently stirring the precursor solution prepared in the step A at room temperature to obtain a spinning solution;
C. b, performing electrostatic spinning on the spinning solution in the step B to obtain a PVC film, and applying a constant-temperature thermal field in a spinning interval and controlling the temperature of a receiving device during the electrostatic spinning;
D. c, drying the PVC film obtained in the step C at room temperature;
E. d, soaking the PVC film obtained in the step D in polyoxometallate solution with a synergistic flame-retardant effect for 10-60min;
F. and E, drying the POM modified PVC film obtained in the step E in a vacuum furnace.
Preferably, the precursor solution according to the step A consists of PVC and a flame-retardant smoke-suppressing agent, the PVC dosage is 10-40% w/v, the flame-retardant smoke-suppressing agent system concentration is 1-5%, and the flame-retardant smoke-suppressing agent is zinc hydroxystannate and an intumescent flame retardant.
Preferably, the precursor solution according to step B is vigorously stirred at room temperature for 12h to 36h.
Preferably, the temperature of the constant temperature thermal field according to the step C is 50-100 ℃, the temperature of the receiving device is-10 ℃ -0 ℃, and the parameters of the electrostatic spinning are as follows: relative humidity 20-70%, perfusion speed 0.4-3mL/h, voltage 10-60kV, distance between receiving device and spinneret orifice 10-40cm, the receiving device is aluminum foil paper or metal plate.
Preferably, the DPVC film according to step is dried at room temperature 40 ℃ for 6h to 24h.
Preferably, the polyoxometallate according to step E is an organic-inorganic heteropolymolybdate, the polyoxometallate being used in an amount of 1-5 wt.%.
Preferably, the POM modified PVC film obtained in the step E is dried in a vacuum oven at 30-60 ℃ for 12-48h according to the step F.
Compared with the prior art, the invention has the beneficial effects that:
the inorganic flame retardant used in the preparation of the flame-retardant smoke-suppressing PVC film has the advantages of high safety, smoke suppression, no toxicity, low price and the like, is stable in performance and difficult to volatilize, accords with the energy-saving and environment-friendly idea advocated by the nation, and is matched with polyoxometallate for synergistic flame retardation, so that the flame-retardant smoke-suppressing effect is more obvious.
Detailed Description
The technical solutions in the embodiments of the present invention are 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 of the 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.
The invention provides the following technical scheme: the preparation method of the flame-retardant smoke-suppressing PVC film comprises the following steps:
A. preparing a precursor solution;
B. b, violently stirring the precursor solution prepared in the step A at room temperature to obtain a spinning solution;
C. b, performing electrostatic spinning on the spinning solution in the step B to obtain a PVC film, and applying a constant-temperature thermal field in a spinning interval and controlling the temperature of a receiving device during the electrostatic spinning;
D. c, drying the PVC film obtained in the step C at room temperature;
E. d, soaking the PVC film obtained in the step D in a polyoxometallate solution with a synergistic flame-retardant effect for 10-60min;
F. and E, drying the POM modified PVC film obtained in the step E in a vacuum furnace.
Dissolving zinc hydroxystannate with the system concentration of 1 percent in PVC water solution with the percentage of 10 w/v to obtain precursor solution, wherein the precursor solution consists of PVC and the flame-retardant smoke-suppressing agent, the PVC consumption is 10-40 w/v, the system concentration of the flame-retardant smoke-suppressing agent is 1-5 percent, and the flame-retardant smoke-suppressing agent is zinc hydroxystannate and an intumescent flame retardant.
Violently stirring the prepared precursor solution at room temperature for 12-36 h to obtain spinning solution
Carrying out electrostatic spinning on the spinning solution to obtain a PVC film, applying a constant-temperature thermal field in a spinning interval and controlling the temperature of a receiving device during electrostatic spinning, wherein the temperature of the constant-temperature thermal field is 50-100 ℃, the temperature of the receiving device is-10-0 ℃, and the parameters of the electrostatic spinning are as follows: relative humidity 20-70%, perfusion speed 0.4-3mL/h, voltage 10-60kV, distance between receiving device and spinneret orifice 10-40cm, the receiving device is aluminum foil paper or metal plate.
Drying the obtained PVC film at the room temperature of 40 ℃ for 6h-24h, soaking the PVC film in polyoxometallate solution with a synergistic flame retardant effect for 10-60min, wherein polyoxometallate is organic-inorganic heteropoly molybdate, the consumption of the polyoxometallate is 1-5wt%, and drying the obtained POM modified PVC film in a vacuum furnace at the temperature of 30-60 ℃ for 12-48h.
Example 1, a precursor solution was obtained by dissolving zinc hydroxystannate with a system concentration of 1% in an aqueous solution of PVC with a concentration of 10% w/v, the precursor solution consisting of PVC and a flame-retardant smoke-suppressing agent, the PVC being used in an amount of 10-40% w/v, the flame-retardant smoke-suppressing agent being zinc hydroxystannate, an intumescent flame retardant, the concentration of the flame-retardant smoke-suppressing agent being 1-5%.
Violently stirring the prepared precursor solution at room temperature for 12 hours to obtain spinning solution
Carrying out electrostatic spinning on the spinning solution to obtain a PVC film, applying a constant-temperature thermal field in a spinning interval during electrostatic spinning, and controlling the temperature of a receiving device, wherein the temperature of the constant-temperature thermal field is 60 ℃, the temperature of the receiving device is 0 ℃, and the parameters of the electrostatic spinning are as follows: the relative humidity is 45%, the pouring speed is 3mL/h, the voltage is 15kV, the distance between a receiving device and a spinneret orifice is 15cm, and the receiving device is aluminum foil paper or a metal plate.
Drying the obtained PVC film at the room temperature of 40 ℃ for 8h, soaking the PVC film in polyoxometallate solution with a synergistic flame-retardant effect for 30min, wherein polyoxometallate is organic-inorganic heteropolymolybdate, the using amount of the polyoxometallate is 1wt%, and drying the obtained POM-modified PVC film in a vacuum furnace at the temperature of 40 ℃ for 24h.
Example 2, a precursor solution is obtained by dissolving zinc hydroxystannate with a system concentration of 1% in a 20% w/v aqueous solution of PVC, the precursor solution consists of PVC and a flame-retardant smoke-suppressing agent, the PVC is used in an amount of 10-40% w/v, the flame-retardant smoke-suppressing agent system concentration is 1-5%, and the flame-retardant smoke-suppressing agent is zinc hydroxystannate and an intumescent flame retardant.
Violently stirring the prepared precursor solution at room temperature for 24 hours to obtain spinning solution
Carrying out electrostatic spinning on the spinning solution to obtain a PVC film, applying a constant-temperature thermal field in a spinning interval and controlling the temperature of a receiving device during electrostatic spinning, wherein the temperature of the constant-temperature thermal field is 75 ℃, the temperature of the receiving device is-5 ℃, and the parameters of the electrostatic spinning are as follows: the relative humidity is 45%, the filling speed is 1mL/h, the voltage is 18kV, the distance between a receiving device and a spinning nozzle is 30cm, and the receiving device is aluminum foil paper or a metal plate.
Drying the obtained PVC film at the room temperature of 40 ℃ for 24h, soaking the PVC film in polyoxometallate solution with a synergistic flame retardant effect for 10min, wherein polyoxometallate is organic-inorganic heteropolymolybdate, the using amount of the polyoxometallate is 5wt%, and drying the obtained POM modified PVC film in a vacuum furnace at the temperature of 30 ℃ for 38h.
The technical principle is as follows: the flame-retardant smoke suppressant not only can play a flame-retardant role in a gas phase and a condensed phase at the same time, but also can generate a synergistic effect with a halogen-containing flame retardant or a metal oxide, and after the POMs are soaked in the PVC film and combined with macromolecular organic groups, organic-inorganic hybrid room-temperature ionic liquid can be generated, so that the PVC film has good synergy and simultaneously improves the compatibility of the PVC film in a matrix.
In conclusion, the inorganic flame retardant used for preparing the flame-retardant smoke-suppressing PVC film has the advantages of high safety, smoke suppression, no toxicity, low price and the like, has stable performance and difficult volatilization, accords with the energy-saving and environment-friendly idea advocated by the nation, and is matched with polyoxometallate for synergistic flame retardation, so that the flame-retardant smoke-suppressing effect is more obvious.
The invention has the beneficial effects that:
the inorganic flame retardant used in the preparation of the flame-retardant smoke-suppressing PVC film has the advantages of high safety, smoke suppression, no toxicity, low price and the like, is stable in performance and difficult to volatilize, accords with the energy-saving and environment-friendly idea advocated by the nation, and is matched with polyoxometallate for synergistic flame retardation, so that the flame-retardant smoke-suppressing effect is more obvious.
Although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that changes, modifications, substitutions and alterations can be made in these embodiments without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.
Claims (3)
1. The preparation method of the flame-retardant smoke-suppressing PVC film is characterized by comprising the following steps: the method comprises the following steps:
A. preparing a precursor solution;
B. b, violently stirring the precursor solution prepared in the step A at room temperature to obtain a spinning solution;
C. b, performing electrostatic spinning on the spinning solution in the step B to obtain a PVC film, and applying a constant-temperature thermal field in a spinning interval and controlling the temperature of a receiving device during the electrostatic spinning;
D. c, drying the PVC film obtained in the step C at room temperature;
E. d, soaking the PVC film obtained in the step D in a polyoxometallate solution with a synergistic flame-retardant effect for 10-60min;
F. drying the PVC film modified by polyoxometallate obtained in the step E in a vacuum furnace;
the precursor solution according to the step A consists of PVC and a flame-retardant smoke suppressant, wherein the using amount of the PVC is 10-40% w/v, the concentration of the flame-retardant smoke suppressant system is 1-5%, and the flame-retardant smoke suppressant is zinc hydroxystannate;
the temperature of the constant-temperature thermal field is 50-100 ℃ according to the step C, the temperature of the receiving device is-10 ℃ -0 ℃, and the parameters of electrostatic spinning are as follows: the relative humidity is 20-70%, the pouring speed is 0.4-3mL/h, the voltage is 10-60kV, the distance between a receiving device and a spinneret orifice is 10-40cm, and the receiving device is aluminum foil paper or a metal plate;
according to the step E, the polyoxometallate is organic-inorganic heteropolymolybdate, and the consumption of the polyoxometallate is 1-5wt%.
2. The preparation of a flame-retardant smoke-suppressing PVC film according to claim 1, wherein: and B, vigorously stirring the precursor solution at room temperature for 12-36 h.
3. The preparation of the flame-retardant and smoke-suppressing PVC film according to claim 1, which is characterized in that: and D, drying the PVC film modified by polyoxometallate obtained in the step E in a vacuum furnace at the temperature of 30-60 ℃ for 12-48h according to the step F.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201911248029.0A CN111041816B (en) | 2019-12-09 | 2019-12-09 | Preparation of flame-retardant smoke-inhibiting PVC film |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201911248029.0A CN111041816B (en) | 2019-12-09 | 2019-12-09 | Preparation of flame-retardant smoke-inhibiting PVC film |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN111041816A CN111041816A (en) | 2020-04-21 |
| CN111041816B true CN111041816B (en) | 2022-10-18 |
Family
ID=70235084
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201911248029.0A Active CN111041816B (en) | 2019-12-09 | 2019-12-09 | Preparation of flame-retardant smoke-inhibiting PVC film |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN111041816B (en) |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112227068A (en) * | 2020-08-24 | 2021-01-15 | 南通花园布业有限公司 | Preparation method of flame-retardant yarn based on polyoxometallate |
Family Cites Families (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3575898A (en) * | 1968-06-20 | 1971-04-20 | Beaunit Corp | Polyvinyl chloride-antimony oxide flame-retardant mixtures for cellulosic spinning dopes |
| DE2847423A1 (en) * | 1978-11-02 | 1980-05-22 | Hoechst Ag | Plastic fuel pipes - with corrugated polyoxymethylene or polyester inner and a flexible PVC sheath |
| US9045845B2 (en) * | 2001-12-28 | 2015-06-02 | Chavanoz Industrie | Composite yarn, method for obtaining same and resulting textile structure |
| CN102505185B (en) * | 2011-09-29 | 2013-08-07 | 东北师范大学 | Method for preparing polyoxometallate composite mesoporous material by electrostatic spinning |
| CN102515185B (en) * | 2011-12-08 | 2014-02-05 | 西北师范大学 | Zinc hydroxystannate-palygorskite clay compound, its preparation and application as fire retardant |
| CN103469353A (en) * | 2013-09-07 | 2013-12-25 | 河北联合大学 | Preparation method of phosphomolybdic acid/polyacrylic acid/polyvinyl alcohol composite fiber |
| CN107377006B (en) * | 2017-08-08 | 2019-10-29 | 东华大学 | A kind of flexibility black TiO2Nano fibrous membrane and preparation method thereof |
| CN109183186A (en) * | 2018-07-16 | 2019-01-11 | 苏州联畅特种纤维有限公司 | A kind of preparation method for the polyurethane fiber that flame retardant property is good |
-
2019
- 2019-12-09 CN CN201911248029.0A patent/CN111041816B/en active Active
Also Published As
| Publication number | Publication date |
|---|---|
| CN111041816A (en) | 2020-04-21 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN103467971B (en) | High-flame-retardance and high-weather-resistance modified polyurethane cable material and preparation method thereof | |
| CN103382676B (en) | A kind of containing rare earth hydrotalcite fire retardant papers and its preparation method and application | |
| CN106633189B (en) | A kind of efficient water resistance expanding fire retardant and its application in polypropylene | |
| CN111041816B (en) | Preparation of flame-retardant smoke-inhibiting PVC film | |
| CN103951870A (en) | Preparation method of phosphor-nitrogen-containing polyelectrolyte complex flame-retardant EVA (ethylene vinyl acetate) | |
| CN107236352B (en) | Aqueous coating film-forming additive composition and preparation method thereof | |
| CN112812368B (en) | Antibacterial flame-retardant material and application method thereof | |
| CN111100310A (en) | Full-biodegradable high-water-resistance film and preparation method and application thereof | |
| CN104877251A (en) | Environment-friendly, low-smoke and lead-free PVC electrical tube and preparation method thereof | |
| CN110016130A (en) | The preparation method of phosphorus, nitrogen type flame retardant and flame-retardant textile based on hyper-branched polyester | |
| KR970021139A (en) | Process for preparing polymer powder redispersible in an aqueous medium | |
| CN103642330B (en) | A kind of cable frie retardant coating | |
| CN109208114B (en) | Flame-retardant antibacterial PET (polyethylene terephthalate) fiber and slice spinning preparation method thereof | |
| CN110845783A (en) | Low-smoke halogen-free flame-retardant polyolefin wire material for B1-grade wire distribution and preparation method thereof | |
| CN105256584A (en) | Antibacterial and flame retardant coating for fabric | |
| CN105110357A (en) | Method used for preparing magnesium hydroxide fire retardant from magnesium salt | |
| CN102702827A (en) | Multifunctional putty for building | |
| CN110358141A (en) | A kind of preparation method of fire retardant high molecular material | |
| CN104262777A (en) | Flame-retardant polypropylene of nano allophane synergistic intumescent flame retardant and preparation method of flame-retardant polypropylene | |
| CN103627263A (en) | Highly chlorinated polyethylene fireproof coating | |
| CN107418330A (en) | A kind of novel heat insulation insulating moulding coating and preparation method thereof | |
| CN115070891B (en) | In-situ self-assembled heteropolyacid hybrid amine nanometer flame retardant in bamboo and wood and preparation method thereof | |
| CN102241852B (en) | EVA fire retardant and its preparation method | |
| CN108034158A (en) | A kind of flame resistant cable material | |
| CN116478615B (en) | Transparent flame-retardant early-warning water-based paint and preparation method and application thereof |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |