CN114523742B - Normal-temperature blended three-proofing filter bag and preparation method thereof - Google Patents

Normal-temperature blended three-proofing filter bag and preparation method thereof Download PDF

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CN114523742B
CN114523742B CN202210118816.9A CN202210118816A CN114523742B CN 114523742 B CN114523742 B CN 114523742B CN 202210118816 A CN202210118816 A CN 202210118816A CN 114523742 B CN114523742 B CN 114523742B
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filter bag
proofing
stirring
hybrid
normal
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CN114523742A (en
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徐清清
充荣强
杨文军
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Guangde Huilong Environmental Protection Technology Co ltd
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Guangde Huilong Environmental Protection Technology Co ltd
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    • D06M15/00Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment
    • D06M15/19Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment with synthetic macromolecular compounds
    • D06M15/21Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
    • D06M15/263Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds of unsaturated carboxylic acids; Salts or esters thereof
    • D06M15/277Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds of unsaturated carboxylic acids; Salts or esters thereof containing fluorine
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B32LAYERED PRODUCTS
    • B32BLAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B5/00Layered products characterised by the non- homogeneity or physical structure, i.e. comprising a fibrous, filamentary, particulate or foam layer; Layered products characterised by having a layer differing constitutionally or physically in different parts
    • B32B5/02Layered products characterised by the non- homogeneity or physical structure, i.e. comprising a fibrous, filamentary, particulate or foam layer; Layered products characterised by having a layer differing constitutionally or physically in different parts characterised by structural features of a fibrous or filamentary layer
    • B32B5/022Non-woven fabric
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    • B32LAYERED PRODUCTS
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    • B32B5/00Layered products characterised by the non- homogeneity or physical structure, i.e. comprising a fibrous, filamentary, particulate or foam layer; Layered products characterised by having a layer differing constitutionally or physically in different parts
    • B32B5/02Layered products characterised by the non- homogeneity or physical structure, i.e. comprising a fibrous, filamentary, particulate or foam layer; Layered products characterised by having a layer differing constitutionally or physically in different parts characterised by structural features of a fibrous or filamentary layer
    • B32B5/08Layered products characterised by the non- homogeneity or physical structure, i.e. comprising a fibrous, filamentary, particulate or foam layer; Layered products characterised by having a layer differing constitutionally or physically in different parts characterised by structural features of a fibrous or filamentary layer the fibres or filaments of a layer being of different substances, e.g. conjugate fibres, mixture of different fibres
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B32LAYERED PRODUCTS
    • B32BLAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B5/00Layered products characterised by the non- homogeneity or physical structure, i.e. comprising a fibrous, filamentary, particulate or foam layer; Layered products characterised by having a layer differing constitutionally or physically in different parts
    • B32B5/22Layered products characterised by the non- homogeneity or physical structure, i.e. comprising a fibrous, filamentary, particulate or foam layer; Layered products characterised by having a layer differing constitutionally or physically in different parts characterised by the presence of two or more layers which are next to each other and are fibrous, filamentary, formed of particles or foamed
    • B32B5/24Layered products characterised by the non- homogeneity or physical structure, i.e. comprising a fibrous, filamentary, particulate or foam layer; Layered products characterised by having a layer differing constitutionally or physically in different parts characterised by the presence of two or more layers which are next to each other and are fibrous, filamentary, formed of particles or foamed one layer being a fibrous or filamentary layer
    • B32B5/26Layered products characterised by the non- homogeneity or physical structure, i.e. comprising a fibrous, filamentary, particulate or foam layer; Layered products characterised by having a layer differing constitutionally or physically in different parts characterised by the presence of two or more layers which are next to each other and are fibrous, filamentary, formed of particles or foamed one layer being a fibrous or filamentary layer another layer next to it also being fibrous or filamentary
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    • D06M11/00Treating 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
    • D06M11/32Treating 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
    • D06M11/36Treating 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
    • D06M11/49Oxides or hydroxides of elements of Groups 8, 9,10 or 18 of the Periodic Table; Ferrates; Cobaltates; Nickelates; Ruthenates; Osmates; Rhodates; Iridates; Palladates; Platinates
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    • D06M11/00Treating 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
    • D06M11/73Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with carbon or compounds thereof
    • D06M11/74Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with carbon or compounds thereof with carbon or graphite; with carbides; with graphitic acids or their salts
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    • D06M15/19Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment with synthetic macromolecular compounds
    • D06M15/21Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
    • D06M15/263Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds of unsaturated carboxylic acids; Salts or esters thereof
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    • D06M15/00Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment
    • D06M15/19Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment with synthetic macromolecular compounds
    • D06M15/21Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
    • D06M15/356Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds of other unsaturated compounds containing nitrogen, sulfur, silicon or phosphorus atoms
    • D06M15/3562Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds of other unsaturated compounds containing nitrogen, sulfur, silicon or phosphorus atoms containing nitrogen
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B32LAYERED PRODUCTS
    • B32BLAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B2262/00Composition or structural features of fibres which form a fibrous or filamentary layer or are present as additives
    • B32B2262/02Synthetic macromolecular fibres
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B32LAYERED PRODUCTS
    • B32BLAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B2262/00Composition or structural features of fibres which form a fibrous or filamentary layer or are present as additives
    • B32B2262/02Synthetic macromolecular fibres
    • B32B2262/0253Polyolefin fibres
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B32LAYERED PRODUCTS
    • B32BLAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B2262/00Composition or structural features of fibres which form a fibrous or filamentary layer or are present as additives
    • B32B2262/02Synthetic macromolecular fibres
    • B32B2262/0276Polyester fibres
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B32LAYERED PRODUCTS
    • B32BLAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B2262/00Composition or structural features of fibres which form a fibrous or filamentary layer or are present as additives
    • B32B2262/02Synthetic macromolecular fibres
    • B32B2262/0276Polyester fibres
    • B32B2262/0284Polyethylene terephthalate [PET] or polybutylene terephthalate [PBT]
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B32LAYERED PRODUCTS
    • B32BLAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B2262/00Composition or structural features of fibres which form a fibrous or filamentary layer or are present as additives
    • B32B2262/10Inorganic fibres
    • BPERFORMING OPERATIONS; TRANSPORTING
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    • B32BLAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B2262/00Composition or structural features of fibres which form a fibrous or filamentary layer or are present as additives
    • B32B2262/14Mixture of at least two fibres made of different materials
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B32LAYERED PRODUCTS
    • B32BLAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B2307/00Properties of the layers or laminate
    • B32B2307/20Properties of the layers or laminate having particular electrical or magnetic properties, e.g. piezoelectric
    • B32B2307/21Anti-static
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B32LAYERED PRODUCTS
    • B32BLAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B2307/00Properties of the layers or laminate
    • B32B2307/30Properties of the layers or laminate having particular thermal properties
    • B32B2307/306Resistant to heat
    • B32B2307/3065Flame resistant or retardant, fire resistant or retardant
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B32LAYERED PRODUCTS
    • B32BLAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B2307/00Properties of the layers or laminate
    • B32B2307/50Properties of the layers or laminate having particular mechanical properties
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    • D06M2101/00Chemical constitution of the fibres, threads, yarns, fabrics or fibrous goods made from such materials, to be treated
    • D06M2101/16Synthetic fibres, other than mineral fibres
    • D06M2101/18Synthetic fibres consisting of macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
    • D06M2101/22Polymers or copolymers of halogenated mono-olefins
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    • D06M2101/16Synthetic fibres, other than mineral fibres
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    • D06M2101/16Synthetic fibres, other than mineral fibres
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    • D06M2200/00Functionality of the treatment composition and/or properties imparted to the textile material
    • D06M2200/10Repellency against liquids
    • D06M2200/11Oleophobic properties
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    • D06M2200/30Flame or heat resistance, fire retardancy properties
    • YGENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02ATECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE
    • Y02A50/00TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE in human health protection, e.g. against extreme weather
    • Y02A50/20Air quality improvement or preservation, e.g. vehicle emission control or emission reduction by using catalytic converters
    • Y02A50/2351Atmospheric particulate matter [PM], e.g. carbon smoke microparticles, smog, aerosol particles, dust

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  • Engineering & Computer Science (AREA)
  • Textile Engineering (AREA)
  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Filtering Materials (AREA)
  • Treatments For Attaching Organic Compounds To Fibrous Goods (AREA)

Abstract

The invention relates to a normal-temperature blended three-proofing filter bag and a preparation method thereof, belonging to the technical field of dust-proofing filter bag preparation, wherein the preparation process is as follows: firstly, paving fiber nets subjected to opening treatment on two sides of a base fabric, and compositing the fiber nets on the base fabric by using a needling process to obtain a filter bag fabric; and secondly, mixing the three-proofing finishing agent with water to soak the filter bag fabric, performing two-soaking and two-rolling, pre-drying for 8-12min at 150-170 ℃, then drying for 4-6h at 180-200 ℃, cutting and sewing to obtain a normal-temperature blended three-proofing filter bag, adding hybrid particles and a polymerization monomer, and preparing the high-efficiency three-proofing finishing agent by an emulsion polymerization method, wherein the three-proofing finishing agent is used in the filter bag, so that the three-proofing filter bag has high water-repellent, oil-repellent and antistatic properties and excellent flame retardant property and mechanical property.

Description

Normal-temperature blended three-proofing filter bag and preparation method thereof
Technical Field
The invention belongs to the technical field of dust-proof filter bag preparation, and particularly relates to a normal-temperature blended three-proof filter bag and a preparation method thereof.
Background
Along with the continuous improvement of environmental protection requirements, some factories with exhaust gas and dust emission increasingly pay attention to environmental protection, when the industrial dust concentration reaches a certain degree (namely explosion limit), if factors such as electrostatic discharge spark or external ignition are met, explosion and fire disaster are extremely easy to cause, so that dust is reduced by arranging a dust remover in the factories, but air dust in the operation of the dust remover contains more moisture and oil, hygroscopicity and easily-soluble dust, ash cleaning difficulty occurs, and therefore, the three-protection filter bag is provided, combines the advantages of water resistance, oil resistance and static resistance, and has higher practicability compared with common filter materials.
The existing three-prevention filter bag has no flame retardant property, dust-containing air generated by some special factories contains combustible gases such as hydrogen, carbon monoxide, methane, acetylene and the like or dust such as grains, aluminum and the like in a concentration range, and can generate severe explosion when meeting a fire source, so that the flame-retardant and antistatic dust-collecting cloth bag is particularly needed.
Disclosure of Invention
In order to solve the technical problems in the background art, the invention provides a normal-temperature blended three-proofing filter bag and a preparation method thereof.
The aim of the invention can be achieved by the following technical scheme:
The normal temperature blending three-proofing filter bag comprises a base cloth layer and a fiber web layer, wherein the fiber web layers are respectively arranged at two sides of the base cloth layer, and the fiber web is compounded at two sides of the base cloth layer through a needling process, so that a sandwich structure is formed;
the normal temperature blending three-proofing filter bag is prepared by the following steps:
Firstly, laying a plurality of layers of fiber webs subjected to opening treatment on two sides of a base fabric, wherein the thickness of the fiber webs is 0.5-1.7mm, and then compositing the fiber webs on the base fabric through a needling process to obtain a filter bag fabric;
Secondly, mixing the three-proofing finishing agent and water according to 150g:1L of the mixture is evenly mixed and then is placed in a trough of a padding machine according to a bath ratio of 1:20, soaking the filter bag fabric by a padding machine, and performing secondary padding to obtain a three-proofing filter material, wherein the padding residual rate is 30-40%, and the padding speed is 4-8m/min;
and thirdly, pre-baking the three-proofing filter material at 150-170 ℃ for 8-12min, then drying at 180-200 ℃ for 4-6h, and then cutting and sewing to obtain the normal-temperature blended three-proofing filter bag.
Further, the three-proofing finishing agent is prepared by the following steps:
S11, mixing hexafluorobutyl methacrylate, N-vinyl pyrrolidone, polyethylene glycol acrylic ester, butyl acrylate and hybrid particles, adding an emulsifier, and stirring for 20-30min at the rotating speed of 300-500r/min to obtain a pre-emulsion;
And S12, adding the 1/4 pre-emulsion, the 1/3 initiator solution and sodium bicarbonate into a reaction kettle, heating to 75 ℃ under the protection of nitrogen, stirring and reacting for 4 hours, then adding the rest pre-emulsion and the initiator solution, heating to 85 ℃, stirring and reacting for 0.5 hour, cooling to room temperature, and regulating the pH value to 6-7 to obtain the three-proofing finishing agent.
Wherein, the mass ratio of the hexafluorobutyl methacrylate to the N-vinyl pyrrolidone to the polyethylene glycol acrylate to the butyl acrylate to the hybrid particles is 60:10-15:10:25:5-8, wherein the emulsifier is prepared from cetyl trimethyl ammonium chloride and fatty alcohol polyoxyethylene ether according to a mass ratio of 2:3, mixing to obtain an initiator solution, wherein the initiator solution is an ammonium persulfate aqueous solution with the mass fraction of 10%, the use level of the emulsifier is 4% of the total mass of hexafluorobutyl methacrylate, N-vinyl pyrrolidone, polyethylene glycol acrylic ester, butyl acrylate and hybrid particles, and the use level of the ammonium persulfate is 0.4% of the total mass of hexafluorobutyl methacrylate, N-vinyl pyrrolidone, polyethylene glycol acrylic ester, butyl acrylate and hybrid particles.
The hybrid particles are made by the steps of:
Step A1, adding hexachlorocyclotriphosphazene, 2-allyl-3-hydroxybenzaldehyde, potassium carbonate and tetrahydrofuran into a three-neck flask, heating to reflux for 48 hours, concentrating a reaction product to 1/4 of the original volume by using a rotary evaporator after the reaction is finished, pouring the reaction product into distilled water, standing for 4-6 hours, carrying out suction filtration, washing a filter cake with distilled water for 3-5 times, and drying to constant weight at 80 ℃ to obtain a flame-retardant monomer;
Wherein, the dosage ratio of hexachlorocyclotriphosphazene, 2-allyl-3-hydroxybenzaldehyde, potassium carbonate and tetrahydrofuran is 5g:0.1mol:9.95g:200-250mL, utilizing hexachlorocyclotriphosphazene and 2-allyl-3-hydroxybenzaldehyde to carry out elimination HCl reaction to obtain a flame retardant monomer;
Step A2, dispersing graphene oxide, feCl 326H2 O and ZnCl 2 into ethylene glycol, performing ultrasonic treatment for 2 hours, adding sodium acetate and polyethylene glycol-400, stirring for 30-40 minutes, transferring into a polytetrafluoroethylene high-pressure reaction kettle, reacting for 10-12 hours at 200 ℃, after the reaction is finished, performing suction filtration on a reaction product, washing a filter cake with distilled water and absolute ethyl alcohol for one time respectively, and finally drying in a 60 ℃ oven until the weight is constant to obtain a nano hybrid;
Wherein, the dosage ratio of graphene oxide, feCl 326H2O、ZnCl2, ethylene glycol, sodium acetate and polyethylene glycol-400 is 30mg:2mmol:1mmol:150-180mL:16.2-16.5g:4.5g, adsorbing zinc and iron metal ions by using graphene oxide with rich carboxyl and other functional groups on the surface as a growth site through electrostatic action, and forming mesoporous zinc ferrite by the iron and zinc metal ions under the action of sodium acetate in the hydrothermal synthesis process and uniformly modifying the mesoporous zinc ferrite on the surface of the graphene oxide to obtain a nano hybrid;
step A3, adding a flame-retardant monomer and tetrahydrofuran into a flask, heating to 40 ℃, stirring for 20-30min, then adding KH-550 and glacial acetic acid, heating to 70 ℃, stirring and reacting for 1h, then adding an ethanol solution of a nano hybrid, cooling to 50 ℃, stirring and reacting for 30-50min, cooling to room temperature after the reaction is finished, centrifuging for 10min at the speed of 9000r/min, removing upper liquid, taking out a centrifuged product, washing for 3-5 times by using the ethanol solution with the mass fraction of 35%, and finally drying for 48h at the temperature of 60 ℃ to obtain hybrid particles;
Wherein, the dosage ratio of the ethanol solution of the flame-retardant monomer, tetrahydrofuran, KH-550, glacial acetic acid and the nanometer hybrid is 0.05mol:180-220mL:0.05mol:1.84mL:60mL of ethanol solution of the nanometer hybrid is prepared from the nanometer hybrid and 50% ethanol solution according to the mass fraction of 18.5-20.3g:60mL ultrasonic mixing; firstly, utilizing aldehyde group of flame-retardant monomer to make condensation reaction with amino group of HK-550, then utilizing siloxane group of HK-550 and hydroxyl group on the surface of nano hybrid to make grafting reaction so as to obtain the invented hybrid particle.
The flame-retardant monomer is prepared by eliminating HCl from hexachlorocyclotriphosphazene and 2-allyl-3-hydroxybenzaldehyde, graphene oxide, feCl 326H2 O and ZnCl 2 are used as raw materials to prepare a nano hybrid, then KH-550 is used as a bridge, the flame-retardant monomer is grafted on the surface of the nano hybrid to obtain hybrid particles, and the hybrid particles not only have good dispersion characteristics, but also contain unsaturated double bond structures and can participate in polymerization reaction, so that the hybrid particles are added into the three-proofing finishing agent, not only can play a role in resisting temperature and flame, but also have a blocking enhancement performance, on one hand, the unique two-dimensional layered structure of the graphene oxide is used for forming a compact continuous uniform carbon layer in the combustion decomposition process, so that the more effective carbon layer blocking effect is utilized to delay heat transfer and the transfer of combustible gas and oxygen in the combustion process, and meanwhile, the oxygen-containing functional groups on the surface of the graphene oxide are used as mesoporous zinc ferrite growth sites, so that the dispersibility of zinc ferrite in a matrix can be improved, the graphene oxide itself can be prevented from dropping down in a pre-formed, and the phenomenon of carbon emulsion can be prevented, and the self-dripping of combustible gas can be prevented.
Further, the base cloth is polyester needled felt, and the fiber net is formed by PPS fiber, basalt fiber, polyester fiber and polytetrafluoroethylene fiber according to the mass ratio of 1:3:1: the PPS fiber, basalt fiber, polyester fiber and polytetrafluoroethylene fiber are prepared according to the warp and weft yarn process, and the fineness of the PPS fiber, basalt fiber, polyester fiber and polytetrafluoroethylene fiber is below 0.4 denier.
The invention has the beneficial effects that:
According to the invention, the three-proofing filter bag with a sandwich structure is obtained by compounding the base cloth layer and the fiber net layer; the tri-proof filter bag has high water repellency, oil repellency and antistatic performance, and also has excellent flame retardant performance and mechanical property, and is mainly due to the fact that the tri-proof finishing agent is obtained by polymerization reaction of hexafluorobutyl methacrylate, N-vinyl pyrrolidone, polyethylene glycol acrylic ester, butyl acrylate and hybrid particles, and has the waterproof, oil repellency and antistatic performance, wherein the addition of the hybrid particles endows the tri-proof finishing agent with excellent flame retardant performance and barrier performance, and the N-vinyl pyrrolidone is polymerized in the tri-proof finishing agent to form a polypyrrole structure, and the polypyrrole structure and the hybrid particles cooperatively play an antistatic role.
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.
Example 1
The embodiment provides a three-proofing finishing agent, which is prepared by the following steps:
Step S11, mixing 60g of hexafluorobutyl methacrylate, 10g of N-vinyl pyrrolidone, 10g of polyethylene glycol acrylic ester, 25g of butyl acrylate and 5g of hybrid particles, adding an emulsifier, and stirring for 20min at the rotating speed of 300r/min to obtain a pre-emulsion;
S12, adding 1/4 of the pre-emulsion, 1/3 of the initiator solution and sodium bicarbonate into a reaction kettle, heating to 75 ℃ under the protection of nitrogen, stirring and reacting for 4 hours, then adding the rest of the pre-emulsion and the initiator solution, heating to 85 ℃, stirring and reacting for 0.5 hour, cooling to room temperature, regulating the pH value to 6, and obtaining the three-proofing finishing agent, wherein the emulsifier is prepared from hexadecyl trimethyl ammonium chloride and fatty alcohol polyoxyethylene ether according to the mass ratio of 2:3, mixing to obtain an initiator solution, wherein the initiator solution is an ammonium persulfate aqueous solution with the mass fraction of 10%, the using amount of the emulsifier is 4% of the total mass of hexafluorobutyl methacrylate, N-vinyl pyrrolidone, polyethylene glycol acrylic ester, butyl acrylate and hybrid particles, and the using amount of the ammonium persulfate is 1/10 of the mass of the initiator.
The hybrid particles are made by the steps of:
Step A1, adding 5g of hexachlorocyclotriphosphazene, 0.1mol of 2-allyl-3-hydroxybenzaldehyde, 9.95g of potassium carbonate and 200mL of tetrahydrofuran into a three-neck flask, heating to reflux for 48h, concentrating a reaction product to 1/4 of the original volume by a rotary evaporator after the reaction is finished, pouring the reaction product into distilled water, standing for 4h, carrying out suction filtration, washing a filter cake with distilled water for 3 times, and drying at 80 ℃ to constant weight to obtain a flame-retardant monomer;
step A2, dispersing 30mg of graphene oxide, 2mmol of FeCl 326H2 O and 1mmol of ZnCl 2 into 150mL of ethylene glycol, performing ultrasonic treatment for 2 hours, adding 16.2g of sodium acetate and 4.5g of polyethylene glycol-400, stirring for 30 minutes, transferring into a polytetrafluoroethylene high-pressure reaction kettle, reacting for 10 hours at 200 ℃, after the reaction is finished, performing suction filtration on a reaction product, washing a filter cake with distilled water and absolute ethyl alcohol for one time respectively, and finally drying in a 60 ℃ oven until the weight is constant to obtain a nano hybrid;
Step A3, adding 0.05mol of flame-retardant monomer and 180mL of tetrahydrofuran into a flask, heating to 40 ℃, stirring for 20min, then adding 0.05mol of KH-550 and 1.84mL of glacial acetic acid, heating to 70 ℃, stirring and reacting for 1h, then adding 60mL of ethanol solution of the nano-hybrid, cooling to 50 ℃, stirring and reacting for 30min, cooling to room temperature after the reaction is finished, centrifuging for 10min under the condition of 9000r/min, removing upper liquid, taking out the centrifuged product, washing 3 times with ethanol solution with the mass fraction of 35%, and finally drying at 60 ℃ for 48h to obtain hybrid particles, wherein the ethanol solution of the nano-hybrid is prepared from the nano-hybrid and ethanol solution with the mass fraction of 50% according to 18.5g:60mL of ultrasonic mixing.
Example 2
The embodiment provides a three-proofing finishing agent, which is prepared by the following steps:
Step S11, mixing 60g of hexafluorobutyl methacrylate, 12g of N-vinyl pyrrolidone, 10g of polyethylene glycol acrylic ester, 25g of butyl acrylate and 7g of hybrid particles, adding an emulsifier, and stirring for 25min at the rotating speed of 400r/min to obtain a pre-emulsion;
S12, adding 1/4 of the pre-emulsion, 1/3 of the initiator solution and sodium bicarbonate into a reaction kettle, heating to 75 ℃ under the protection of nitrogen, stirring and reacting for 4 hours, then adding the rest of the pre-emulsion and the initiator solution, heating to 85 ℃, stirring and reacting for 0.5 hour, cooling to room temperature, regulating the pH value to 6, and obtaining the three-proofing finishing agent, wherein the emulsifier is prepared from hexadecyl trimethyl ammonium chloride and fatty alcohol polyoxyethylene ether according to the mass ratio of 2:3, mixing to obtain an initiator solution, wherein the initiator solution is an ammonium persulfate aqueous solution with the mass fraction of 10%, the using amount of the emulsifier is 4% of the total mass of hexafluorobutyl methacrylate, N-vinyl pyrrolidone, polyethylene glycol acrylic ester, butyl acrylate and hybrid particles, and the using amount of the ammonium persulfate is 1/10 of the mass of the initiator.
The hybrid particles are made by the steps of:
step A1, adding 5g of hexachlorocyclotriphosphazene, 0.1mol of 2-allyl-3-hydroxybenzaldehyde, 9.95g of potassium carbonate and 220mL of tetrahydrofuran into a three-neck flask, heating to reflux for 48h, concentrating a reaction product to 1/4 of the original volume by a rotary evaporator after the reaction is finished, pouring the reaction product into distilled water, standing for 5h, carrying out suction filtration, washing a filter cake with distilled water for 4 times, and drying at 80 ℃ to constant weight to obtain a flame-retardant monomer;
step A2, dispersing 30mg of graphene oxide, 2mmol of FeCl 326H2 O and 1mmol of ZnCl 2 into 170mL of ethylene glycol, performing ultrasonic treatment for 2 hours, adding 16.4g of sodium acetate and 4.5g of polyethylene glycol-400, stirring for 35 minutes, transferring into a polytetrafluoroethylene high-pressure reaction kettle, reacting for 11 hours at 200 ℃, after the reaction is finished, performing suction filtration on a reaction product, washing a filter cake with distilled water and absolute ethyl alcohol for one time respectively, and finally drying in a 60 ℃ oven until the weight is constant to obtain a nano hybrid;
Step A3, adding 0.05mol of flame-retardant monomer and 190mL of tetrahydrofuran into a flask, heating to 40 ℃, stirring for 25min, then adding 0.05mol of KH-550 and 1.84mL of glacial acetic acid, heating to 70 ℃, stirring and reacting for 1h, then adding 60mL of ethanol solution of the nano-hybrid, cooling to 50 ℃, stirring and reacting for 40min, cooling to room temperature after the reaction is finished, centrifuging for 10min under the condition of 9000r/min, removing upper liquid, taking out the centrifuged product, washing for 4 times by using ethanol solution with the mass fraction of 35%, and finally drying at 60 ℃ for 48h to obtain hybrid particles, wherein the ethanol solution of the nano-hybrid is prepared by mixing the nano-hybrid and ethanol solution with the mass fraction of 50% according to 19.5g:60mL of ultrasonic mixing.
Example 3
The embodiment provides a three-proofing finishing agent, which is prepared by the following steps:
Step S11, mixing 60g of hexafluorobutyl methacrylate, 15g of N-vinyl pyrrolidone, 10g of polyethylene glycol acrylic ester, 25g of butyl acrylate and 8g of hybrid particles, adding an emulsifier, and stirring for 30min at the rotating speed of 500r/min to obtain a pre-emulsion;
S12, adding 1/4 of the pre-emulsion, 1/3 of the initiator solution and sodium bicarbonate into a reaction kettle, heating to 75 ℃ under the protection of nitrogen, stirring and reacting for 4 hours, then adding the rest of the pre-emulsion and the initiator solution, heating to 85 ℃, stirring and reacting for 0.5 hour, cooling to room temperature, regulating the pH value to 7, and obtaining the three-proofing finishing agent, wherein the emulsifier is prepared from hexadecyl trimethyl ammonium chloride and fatty alcohol polyoxyethylene ether according to the mass ratio of 2:3, mixing to obtain an initiator solution, wherein the initiator solution is an ammonium persulfate aqueous solution with the mass fraction of 10%, the using amount of the emulsifier is 4% of the total mass of hexafluorobutyl methacrylate, N-vinyl pyrrolidone, polyethylene glycol acrylic ester, butyl acrylate and hybrid particles, and the using amount of the ammonium persulfate is 1/10 of the mass of the initiator.
The hybrid particles are made by the steps of:
Step A1, adding 5g of hexachlorocyclotriphosphazene, 0.1mol of 2-allyl-3-hydroxybenzaldehyde, 9.95g of potassium carbonate and 250mL of tetrahydrofuran into a three-neck flask, heating to reflux for 48h, concentrating a reaction product to 1/4 of the original volume by a rotary evaporator after the reaction is finished, pouring the reaction product into distilled water, standing for 6h, carrying out suction filtration, washing a filter cake with distilled water for 5 times, and drying at 80 ℃ to constant weight to obtain a flame-retardant monomer;
Step A2, dispersing 30mg of graphene oxide, 2mmol of FeCl 326H2 O and 1mmol of ZnCl 2 into 180mL of ethylene glycol, performing ultrasonic treatment for 2 hours, adding 16.5g of sodium acetate and 4.5g of polyethylene glycol-400, stirring for 40 minutes, transferring into a polytetrafluoroethylene high-pressure reaction kettle, reacting for 12 hours at 200 ℃, after the reaction is finished, performing suction filtration on a reaction product, washing a filter cake once by distilled water and absolute ethyl alcohol respectively, and finally drying in a 60 ℃ oven until the weight is constant to obtain a nano hybrid;
Step A3, adding 0.05mol of flame-retardant monomer and 220mL of tetrahydrofuran into a flask, heating to 40 ℃, stirring for 30min, then adding 0.05mol of KH-550 and 1.84mL of glacial acetic acid, heating to 70 ℃, stirring and reacting for 1h, then adding 60mL of ethanol solution of the nano-hybrid, cooling to 50 ℃, stirring and reacting for 50min, cooling to room temperature after the reaction is finished, centrifuging for 10min under the condition of 9000r/min, removing upper liquid, taking out the centrifuged product, washing 5 times with ethanol solution with the mass fraction of 35%, and finally drying at 60 ℃ for 48h to obtain hybrid particles, wherein the ethanol solution of the nano-hybrid is prepared by mixing the nano-hybrid and ethanol solution with the mass fraction of 50% according to 20.3g:60mL of ultrasonic mixing.
Comparative example 1
The hybrid particles of example 1 were removed, and the remaining starting materials and preparation process were unchanged.
Comparative example 2
The nano-hybrid in example 2 was replaced with graphene oxide, and the rest of the raw materials and the preparation process were unchanged.
Example 4
The normal temperature blending three-proofing filter bag comprises a base cloth layer and a fiber web layer, wherein the fiber web layers are respectively arranged at two sides of the base cloth layer, and the fiber web is compounded at two sides of the base cloth layer through a needling process, so that a sandwich structure is formed;
the normal temperature blending three-proofing filter bag is prepared by the following steps:
firstly, laying a plurality of layers of fiber nets which are subjected to opening treatment on two sides of a base fabric, wherein the thickness of the fiber nets is 0.5mm, and then compounding the fiber nets on the base fabric through a needling process to obtain a filter bag fabric;
second step, the three-proofing agent of example 1 and water were mixed according to 150g:1L of the mixture is evenly mixed and then is placed in a trough of a padding machine according to a bath ratio of 1:20, soaking the filter bag fabric by a padding machine, and performing secondary padding to obtain a three-proofing filter material, wherein the padding residual rate is 30%, and the padding speed is 4m/min;
And thirdly, pre-baking the three-proofing filter material at 170 ℃ for 12min, then drying at 180 ℃ for 6h, and then cutting and sewing to obtain the normal-temperature blended three-proofing filter bag.
Wherein, the base cloth is polyester needled felt, and the fiber network is formed by PPS fiber, basalt fiber, polyester fiber and polytetrafluoroethylene fiber according to the mass ratio of 1:3:1: the PPS fiber, basalt fiber, polyester fiber and polytetrafluoroethylene fiber are prepared according to the warp and weft yarn process, and the fineness of the PPS fiber, basalt fiber, polyester fiber and polytetrafluoroethylene fiber is below 0.4 denier.
Example 5
The normal temperature blending three-proofing filter bag comprises a base cloth layer and a fiber web layer, wherein the fiber web layers are respectively arranged at two sides of the base cloth layer, and the fiber web is compounded at two sides of the base cloth layer through a needling process, so that a sandwich structure is formed;
the normal temperature blending three-proofing filter bag is prepared by the following steps:
Firstly, laying a plurality of layers of fiber nets which are subjected to opening treatment on two sides of a base fabric, wherein the thickness of the fiber nets is 1.1mm, and then compounding the fiber nets on the base fabric through a needling process to obtain a filter bag fabric;
Second step, the three-proofing agent of example 2 and water were mixed according to 150g:1L of the mixture is evenly mixed and then is placed in a trough of a padding machine according to a bath ratio of 1:20, soaking the filter bag fabric by a padding machine, and performing secondary padding to obtain a three-proofing filter material, wherein the padding residual rate is 35%, and the padding speed is 6m/min;
and thirdly, pre-baking the three-proofing filter material at 160 ℃ for 10min, then drying at 190 ℃ for 5h, and then cutting and sewing to obtain the normal-temperature blended three-proofing filter bag.
Wherein, the base cloth is polyester needled felt, and the fiber network is formed by PPS fiber, basalt fiber, polyester fiber and polytetrafluoroethylene fiber according to the mass ratio of 1:3:1: the PPS fiber, basalt fiber, polyester fiber and polytetrafluoroethylene fiber are prepared according to the warp and weft yarn process, and the fineness of the PPS fiber, basalt fiber, polyester fiber and polytetrafluoroethylene fiber is below 0.4 denier.
Example 6
The normal temperature blending three-proofing filter bag comprises a base cloth layer and a fiber web layer, wherein the fiber web layers are respectively arranged at two sides of the base cloth layer, and the fiber web is compounded at two sides of the base cloth layer through a needling process, so that a sandwich structure is formed;
the normal temperature blending three-proofing filter bag is prepared by the following steps:
Firstly, laying a plurality of layers of fiber nets which are subjected to opening treatment on two sides of a base fabric, wherein the thickness of the fiber nets is 1.7mm, and then compounding the fiber nets on the base fabric through a needling process to obtain a filter bag fabric;
Second step, the three-proofing agent of example 3 and water were mixed according to 150g:1L of the mixture is evenly mixed and then is placed in a trough of a padding machine according to a bath ratio of 1:20, soaking the filter bag fabric by a padding machine, and performing secondary padding to obtain a three-proofing filter material, wherein the padding residual rate is 40%, and the padding speed is 8m/min;
and thirdly, pre-baking the three-proofing filter material for 8min at 150 ℃, then drying for 4h at 200 ℃, and then cutting and sewing to obtain the normal-temperature blended three-proofing filter bag.
Wherein, the base cloth is polyester needled felt, and the fiber network is formed by PPS fiber, basalt fiber, polyester fiber and polytetrafluoroethylene fiber according to the mass ratio of 1:3:1: the PPS fiber, basalt fiber, polyester fiber and polytetrafluoroethylene fiber are prepared according to the warp and weft yarn process, and the fineness of the PPS fiber, basalt fiber, polyester fiber and polytetrafluoroethylene fiber is below 0.4 denier.
Comparative example 3
The three-proofing agent in example 4 was replaced with the three-proofing agent in comparative example 1, and the remaining raw materials and the preparation process were unchanged.
Comparative example 4
The three-proofing agent in example 5 was replaced with the three-proofing agent in comparative example 2, and the remaining raw materials and the preparation process were unchanged.
Comparative example 5
The three-proofing agent in example 6 was replaced with the three-proofing agent sold by Shanghai hong Help Utility Co., ltd, and the rest of the raw materials and the preparation process were unchanged.
The three-proofing filter bags prepared in examples 4 to 6 and comparative examples 3 to 5 were tested as follows:
Water repellency properties: the water repellency performance test is carried out according to the AAT CC 22-2005 'textile water repellency test spray method'. And (3) taking a sample to be tested, clamping the sample to be tested to a flat and tight state by using a clamp, placing the fabric to be tested on a 45-degree inclined plane along the direction of water drops on the cloth surface, and sprinkling the center of the sample to be tested on the surface of the sample within 25-30s by using a spray head at a position 150mm below the center of the surface of the spray nozzle. After showering, the tested samples were rated against the standard, 5 total grades, the worst grade 1, and the best grade 5.
Oil repellency: according to AATCC 118-2007, "oil drainage: the oil repellency test was carried out in the hydrocarbon resistance test standard. The test is preceded by a standing under standard conditions for at least 4 hours. Two samples of 20cm320cm were taken at a distance from the selvedge and the end of the cloth, and the samples were flat and free of creases. At 5 positions on the sample, which were 4cm apart from each other, the droplet diameter was 5mm or the volume was 5mL, and the droplet shape was observed at an angle of about 45 deg. for 30s. Rating was performed according to AATCC118 rating method, worst rating 1, best rating 8.
Air permeability: the method is characterized in that an FX3300 III fabric air permeability tester is adopted, the test is carried out according to DIN EN ISO 9237-1995 "textile fiber fabric air permeability measurement", the test area is 20cm 2, the pressure difference is 200Pa, the air flow which vertically passes through a given area of a sample within a certain time is tested, the samples of different parts of the same fabric are sampled for 10 times, and the average value is obtained.
Combustion performance: according to GB 8410-2006 combustion characteristics of automotive interior materials, horizontal flame retardant performance test is carried out, the temperature (23+/-2) DEG C and relative humidity of a sample before test are adjusted for at least 24 hours but not more than 168 hours in a standard state of 45% -55%, 5 pieces of cloth samples are taken in the warp and weft directions respectively during test, and an average value is obtained. If the sample is exposed to the flame for 15 seconds, the fire source extinguishing sample is still unburned, or the sample can burn, but the flame is extinguished before reaching the first measurement mark, the no burning distance is counted, and the A-0mm/min is recorded. If the experiment timing starts, the flame is automatically extinguished within 60 seconds, and the burning distance is not more than 50mm, the flame is considered to meet the burning speed requirement, and the result is marked as B.
Breaking strength: on a universal stretcher, according to GB/T3923.1-2013 textile fabric tensile Property part 1: determination of breaking Strength and elongation at break (bar sample method) criteria the breaking strength before and after finishing of the fabric was tested, and each sample was tested by taking 5 samples in the warp and weft directions, respectively, and taking the average.
The test results are shown in table 1:
TABLE 1
As can be seen from Table 1, the filter bags prepared in examples 4-6 have high water and oil repellency and good flame retardant and mechanical properties.
Antistatic properties: the test method refers to a specific test method of GB/T24249-2009 antistatic clean fabric, the surface resistivity and the friction electrification voltage of the fabric are calculated, the number of test samples is not less than 5, and a test average value is obtained.
Acid resistance: placing the three-proofing filter bags prepared in the examples 4-6 and the comparative examples 3-5 in hydrochloric acid solution with the mass fraction of 5%, soaking for 48 hours at 60 ℃, and observing whether bubbles, falling off and other phenomena exist;
alkali resistance: placing the three-proofing filter bags prepared in the examples 4-6 and the comparative examples 3-5 in sodium hydroxide solution with the mass fraction of 5%, soaking for 48 hours at 60 ℃, and observing whether bubbles, falling off and other phenomena exist;
The test results are shown in table 2:
TABLE 2
As can be seen from Table 2, the filter bags prepared in examples 4-6 have good antistatic and corrosion resistance properties.
In conclusion, the three-proofing filter bag prepared by the invention has higher water repellency, oil repellency and antistatic performance, and also has higher flame retardance and mechanical property.
In the description of the present specification, the descriptions of the terms "one embodiment," "example," "specific example," and the like, mean that a particular feature, structure, material, or characteristic described in connection with the embodiment or example is included in at least one embodiment or example of the present invention. In this specification, schematic representations of the above terms do not necessarily refer to the same embodiments or examples. Furthermore, the particular features, structures, materials, or characteristics described may be combined in any suitable manner in any one or more embodiments or examples.
The foregoing is merely illustrative and explanatory of the invention, as various modifications and additions may be made to the particular embodiments described, or in a similar manner, by those skilled in the art, without departing from the scope of the invention or exceeding the scope of the invention as defined in the claims.

Claims (5)

1. The preparation method of the normal-temperature blended three-proofing filter bag is characterized by comprising the following steps of:
firstly, paving fiber nets subjected to opening treatment on two sides of a base fabric, and compositing the fiber nets on the base fabric by using a needling process to obtain a filter bag fabric;
Secondly, mixing hexafluorobutyl methacrylate, N-vinyl pyrrolidone, polyethylene glycol acrylic ester, butyl acrylate and hybrid particles, adding an emulsifier, and stirring to obtain a pre-emulsion;
thirdly, mixing 1/4 of the pre-emulsion, 1/3 of the initiator solution and sodium bicarbonate, heating to 75 ℃ under the protection of nitrogen, stirring and reacting for 4 hours, adding the rest of the pre-emulsion and the initiator solution, heating to 85 ℃, stirring and reacting for 0.5 hour, cooling to room temperature, and regulating the pH value to 6-7 to obtain the three-proofing finishing agent;
Fourthly, mixing the three-proofing finishing agent with water to soak the filter bag fabric, performing two-soaking and two-rolling, pre-drying for 8-12min at 150-170 ℃, then drying for 4-6h at 180-200 ℃, and performing cutting and sewing to obtain the normal-temperature blended three-proofing filter bag;
the hybrid particles are made by the steps of:
Adding a flame-retardant monomer and tetrahydrofuran into a flask, heating to 40 ℃ and stirring for 20-30min, adding KH-550 and glacial acetic acid, heating to 70 ℃ and stirring for reaction for 1h, adding an ethanol solution of the nanometer hybrid, cooling to 50 ℃, stirring for reaction for 30-50min, centrifuging, washing and drying to obtain hybrid particles;
the flame-retardant monomer is prepared by the following steps:
Mixing hexachlorocyclotriphosphazene, 2-allyl-3-hydroxybenzaldehyde, potassium carbonate and tetrahydrofuran, carrying out reflux reaction for 48 hours, concentrating to 1/4 of the original volume, then pouring into distilled water, standing for 4-6 hours, carrying out suction filtration, washing a filter cake, and drying to obtain a flame retardant monomer;
the nanometer hybrid is prepared by the following steps:
dispersing graphene oxide, feCl 3·6H2 O and ZnCl 2 into ethylene glycol, performing ultrasonic treatment for 2 hours, adding sodium acetate and polyethylene glycol-400, stirring, transferring to a reaction kettle, reacting for 10-12 hours at 200 ℃, performing suction filtration, washing a filter cake, and drying to obtain the nano hybrid.
2. The preparation method of the normal-temperature blended three-proofing filter bag according to claim 1, which is characterized in that the emulsifier is prepared from cetyl trimethyl ammonium chloride and fatty alcohol polyoxyethylene ether according to a mass ratio of 2:3, mixing to obtain an initiator solution, wherein the initiator solution is an ammonium persulfate aqueous solution with the mass fraction of 10%.
3. The method for preparing the normal-temperature blended three-proofing filter bag according to claim 2, wherein the using amount of the emulsifier is 4% of the total mass of hexafluorobutyl methacrylate, N-vinyl pyrrolidone, polyethylene glycol acrylate, butyl acrylate and hybrid particles, and the using amount of ammonium persulfate is 0.4% of the total mass of hexafluorobutyl methacrylate, N-vinyl pyrrolidone, polyethylene glycol acrylate, butyl acrylate and hybrid particles.
4. The preparation method of the normal-temperature blended three-proofing filter bag according to claim 1, which is characterized in that the ethanol solution of the nanometer hybrid is prepared from 18.5-20.3g of the nanometer hybrid and 50% ethanol solution by mass percent: 60mL of ultrasonic mixing.
5. A normal temperature blended three-proofing filter bag, which is characterized by being prepared by the preparation method of any one of claims 1-4.
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