CN110629561A - Preparation method of antimony-free burn-through-resistant water-based flame retardant adhesive for fabric coating - Google Patents
Preparation method of antimony-free burn-through-resistant water-based flame retardant adhesive for fabric coating Download PDFInfo
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- CN110629561A CN110629561A CN201910731011.XA CN201910731011A CN110629561A CN 110629561 A CN110629561 A CN 110629561A CN 201910731011 A CN201910731011 A CN 201910731011A CN 110629561 A CN110629561 A CN 110629561A
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06N—WALL, FLOOR, OR LIKE COVERING MATERIALS, e.g. LINOLEUM, OILCLOTH, ARTIFICIAL LEATHER, ROOFING FELT, CONSISTING OF A FIBROUS WEB COATED WITH A LAYER OF MACROMOLECULAR MATERIAL; FLEXIBLE SHEET MATERIAL NOT OTHERWISE PROVIDED FOR
- D06N3/00—Artificial leather, oilcloth or other material obtained by covering fibrous webs with macromolecular material, e.g. resins, rubber or derivatives thereof
- D06N3/0056—Artificial leather, oilcloth or other material obtained by covering fibrous webs with macromolecular material, e.g. resins, rubber or derivatives thereof characterised by the compounding ingredients of the macro-molecular coating
- D06N3/0059—Organic ingredients with special effects, e.g. oil- or water-repellent, antimicrobial, flame-resistant, magnetic, bactericidal, odour-influencing agents; perfumes
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06N—WALL, FLOOR, OR LIKE COVERING MATERIALS, e.g. LINOLEUM, OILCLOTH, ARTIFICIAL LEATHER, ROOFING FELT, CONSISTING OF A FIBROUS WEB COATED WITH A LAYER OF MACROMOLECULAR MATERIAL; FLEXIBLE SHEET MATERIAL NOT OTHERWISE PROVIDED FOR
- D06N3/00—Artificial leather, oilcloth or other material obtained by covering fibrous webs with macromolecular material, e.g. resins, rubber or derivatives thereof
- D06N3/0056—Artificial leather, oilcloth or other material obtained by covering fibrous webs with macromolecular material, e.g. resins, rubber or derivatives thereof characterised by the compounding ingredients of the macro-molecular coating
- D06N3/0061—Organic fillers or organic fibrous fillers, e.g. ground leather waste, wood bark, cork powder, vegetable flour; Other organic compounding ingredients; Post-treatment with organic compounds
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06N—WALL, FLOOR, OR LIKE COVERING MATERIALS, e.g. LINOLEUM, OILCLOTH, ARTIFICIAL LEATHER, ROOFING FELT, CONSISTING OF A FIBROUS WEB COATED WITH A LAYER OF MACROMOLECULAR MATERIAL; FLEXIBLE SHEET MATERIAL NOT OTHERWISE PROVIDED FOR
- D06N3/00—Artificial leather, oilcloth or other material obtained by covering fibrous webs with macromolecular material, e.g. resins, rubber or derivatives thereof
- D06N3/0056—Artificial leather, oilcloth or other material obtained by covering fibrous webs with macromolecular material, e.g. resins, rubber or derivatives thereof characterised by the compounding ingredients of the macro-molecular coating
- D06N3/0063—Inorganic compounding ingredients, e.g. metals, carbon fibres, Na2CO3, metal layers; Post-treatment with inorganic compounds
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06N—WALL, FLOOR, OR LIKE COVERING MATERIALS, e.g. LINOLEUM, OILCLOTH, ARTIFICIAL LEATHER, ROOFING FELT, CONSISTING OF A FIBROUS WEB COATED WITH A LAYER OF MACROMOLECULAR MATERIAL; FLEXIBLE SHEET MATERIAL NOT OTHERWISE PROVIDED FOR
- D06N3/00—Artificial leather, oilcloth or other material obtained by covering fibrous webs with macromolecular material, e.g. resins, rubber or derivatives thereof
- D06N3/04—Artificial leather, oilcloth or other material obtained by covering fibrous webs with macromolecular material, e.g. resins, rubber or derivatives thereof with macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06N—WALL, FLOOR, OR LIKE COVERING MATERIALS, e.g. LINOLEUM, OILCLOTH, ARTIFICIAL LEATHER, ROOFING FELT, CONSISTING OF A FIBROUS WEB COATED WITH A LAYER OF MACROMOLECULAR MATERIAL; FLEXIBLE SHEET MATERIAL NOT OTHERWISE PROVIDED FOR
- D06N3/00—Artificial leather, oilcloth or other material obtained by covering fibrous webs with macromolecular material, e.g. resins, rubber or derivatives thereof
- D06N3/04—Artificial leather, oilcloth or other material obtained by covering fibrous webs with macromolecular material, e.g. resins, rubber or derivatives thereof with macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
- D06N3/042—Acrylic polymers
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06N—WALL, FLOOR, OR LIKE COVERING MATERIALS, e.g. LINOLEUM, OILCLOTH, ARTIFICIAL LEATHER, ROOFING FELT, CONSISTING OF A FIBROUS WEB COATED WITH A LAYER OF MACROMOLECULAR MATERIAL; FLEXIBLE SHEET MATERIAL NOT OTHERWISE PROVIDED FOR
- D06N3/00—Artificial leather, oilcloth or other material obtained by covering fibrous webs with macromolecular material, e.g. resins, rubber or derivatives thereof
- D06N3/04—Artificial leather, oilcloth or other material obtained by covering fibrous webs with macromolecular material, e.g. resins, rubber or derivatives thereof with macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
- D06N3/10—Artificial leather, oilcloth or other material obtained by covering fibrous webs with macromolecular material, e.g. resins, rubber or derivatives thereof with macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds with styrene-butadiene copolymerisation products or other synthetic rubbers or elastomers except polyurethanes
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- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06N—WALL, FLOOR, OR LIKE COVERING MATERIALS, e.g. LINOLEUM, OILCLOTH, ARTIFICIAL LEATHER, ROOFING FELT, CONSISTING OF A FIBROUS WEB COATED WITH A LAYER OF MACROMOLECULAR MATERIAL; FLEXIBLE SHEET MATERIAL NOT OTHERWISE PROVIDED FOR
- D06N3/00—Artificial leather, oilcloth or other material obtained by covering fibrous webs with macromolecular material, e.g. resins, rubber or derivatives thereof
- D06N3/12—Artificial leather, oilcloth or other material obtained by covering fibrous webs with macromolecular material, e.g. resins, rubber or derivatives thereof with macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds, e.g. gelatine proteins
- D06N3/14—Artificial leather, oilcloth or other material obtained by covering fibrous webs with macromolecular material, e.g. resins, rubber or derivatives thereof with macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds, e.g. gelatine proteins with polyurethanes
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
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- D06N2209/00—Properties of the materials
- D06N2209/06—Properties of the materials having thermal properties
- D06N2209/067—Flame resistant, fire resistant
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Abstract
The invention belongs to the technical field of water-based flame-retardant adhesive for fabric coatings, and particularly relates to a preparation method of antimony-free burn-through-resistant water-based flame-retardant adhesive for fabric coatings, which comprises the following steps of preparing raw materials, wherein the raw materials comprise 20-40 parts of water-based resin, 20-40 parts of flame retardant, 2-10 parts of polyvinyl alcohol, 0.2-5 parts of auxiliary agent and 5-50 parts of water, and the total weight of the raw materials is 100 parts; preparing a finished product by the processes of preparing a solution of polyvinyl alcohol, preparing a powder flame retardant aqueous dispersion, pretreating a phosphate flame retardant, mixing and filtering; according to the preparation method of the antimony-free burn-through-resistant water-based flame retardant adhesive for the fabric coating, antimony trioxide is not used, and the harm of residual heavy metals in the antimony trioxide to human health is reduced; by arranging the polyvinyl alcohol as the carbon forming agent, the fabric has excellent carbon forming performance, burn-through resistance and anti-dripping performance, and is particularly suitable for fabric flame-retardant coatings of mattresses, sofas, furniture coverings, mattresses, carpets, protective clothing and the like.
Description
Technical Field
The invention relates to the technical field of antimony-free water-based flame retardant adhesives for fabric coatings, in particular to a preparation method of antimony-free burn-through resistant water-based flame retardant adhesives for fabric coatings.
Background
In recent years, with the progress of society and the improvement of the living standard of people, the consumption of various textiles for civil use and industry is rapidly increased, and especially the demand of various indoor decorative fabrics such as curtains, wall cloth, carpets, furniture cloth, bedding, tent cloth and automobile interior decorative fabrics is increased day by day. Meanwhile, the number of fires caused by the fire of textiles is also increasing, resulting in serious economic loss and casualties. Therefore, the textile is subjected to flame retardant treatment, the fire spreading speed is delayed, and the method has great significance for reducing life and property loss.
The traditional water-based flame-retardant adhesive for textile coating mostly contains antimony trioxide. After the flame-retardant adhesive coating of the system is coated on textiles, although the flame-retardant adhesive has certain flame-retardant performance, the flame-retardant adhesive has certain defects:
first, even high-purity antimony trioxide contains a certain amount of heavy metals such as lead and cadmium, and these heavy metals do not contribute to the health of the human body. It is not useful in infant products.
Secondly, the carbon forming property is poor, the polyester fabric is easy to burn through after being coated by the flame-retardant glue, and in the specific application aspect, the sofa is easy to burn through after a fire source contacts the surface of the sofa, so that the sponge filler behind the sofa is ignited, and a fire disaster is caused.
Chinese patent application No. 93115328.. X discloses a flame retardant coating for fabric coating, chinese patent application No. cn20048002553.X discloses a flame retardant for general fabric coating, chinese patent application No. cn101498105.b discloses a flame retardant glue for fabric coating, which is coated on fabric, the fabric is easy to burn through, thereby igniting the sponge covered after the fabric, although the coating amount of the flame retardant glue can be increased to pass the test, the flame retardant cost is higher.
Chinese patent application No. 201610907466.9 discloses a burn-through resistant water-based flame-retardant adhesive for textile, which contains no antimony and is not easy to burn through, but after the water-based flame-retardant adhesive is coated on a fabric and is soaked in water at 40 ℃ for 30 minutes, the flame-retardant property is reduced, the burn-through resistance is greatly reduced, and the burn and scald are easily caused by molten drops.
Disclosure of Invention
Most of the conventional water-based flame-retardant adhesives for textile coatings contain antimony trioxide, and the antimony trioxide contains certain heavy metals such as lead, arsenic and cadmium, and the heavy metals do not utilize the health of human bodies. The invention provides a preparation method of antimony-free burn-through resistant water-based flame retardant adhesive for a fabric coating.
The invention provides a preparation method of antimony-free burn-through-resistant water-based flame retardant adhesive for a fabric coating, which comprises the following steps of preparing raw materials in parts by weight:
the total weight of the raw materials is 100 parts;
step two, preparing a polyvinyl alcohol solution,
adding the polyvinyl alcohol obtained in the step one into a container with a stirring and heating device, adding water with the weight 2-8 times that of the polyvinyl alcohol, slowly stirring until the polyvinyl alcohol is fully dissolved, starting the heating device for the polyvinyl alcohol which is not easily dissolved at normal temperature, raising the temperature to 50-95 ℃, continuously stirring until the polyvinyl alcohol is fully dissolved, then adding the cross-linking agent, the bactericide and the defoaming agent in the auxiliary agent obtained in the step one, and stirring to obtain a polyvinyl alcohol aqueous solution for later use;
step three, preparing the powder flame retardant water dispersion liquid,
adding the balance of the water in the step one and the dispersing agent and the wetting agent in the auxiliary in the step one into a container with a stirring device, and stirring for 1-5 minutes; then adding the powder flame retardant while stirring, increasing the stirring speed to more than 1000 revolutions per minute, continuing stirring, fully dispersing the powder flame retardant in water, and filtering to obtain a powder flame retardant aqueous dispersion for later use;
step four, pre-treating the phosphate flame retardant,
adding one or more phosphate flame retardants in the step one into a container with a stirring and heating device, starting the stirring device, and stirring; after stirring at normal temperature, if solid phosphate flame retardant exists, starting the heating device, and continuing stirring to enable the system to be in a liquid state. Removing impurities to prepare the liquid phosphate flame retardant for later use.
Step five, preparing the flame-retardant adhesive,
adding the rest of water, water-based resin and polyvinyl alcohol solution prepared in the step two into a container with a stirring device, adding the powdery flame retardant aqueous dispersion prepared in the step three, starting a stirrer, slowly stirring for 1-10 minutes, adding the phosphate flame retardant pretreated in the step four, increasing the rotating speed of the stirrer to be more than 1000 revolutions per minute, stirring until the mixture is fully and uniformly mixed, checking the viscosity condition of the mixture, and adding a thickening agent to increase the consistency; and (5) preparing a finished product, discharging and packaging.
Preferably, the aqueous resin in the first step includes one or more of ethylene-vinyl acetate copolymer emulsion, acrylate emulsion, polyurethane emulsion, styrene-butadiene emulsion and butyronitrile emulsion, and the solid content of the aqueous resin is 20% -60%.
Preferably, the flame retardant in the first step comprises Hexabromocyclododecane (HBCD), decabromodiphenyl ether, decabromodiphenylethane, tris (2, 3-dibromopropyl) isocyanurate, bromotriazine, ethylenebistetrabromophthalimide, tetrabromobisphenol A, octabromoether, methyl octabromoether, ammonium polyphosphate (APP), guanidine phosphate, guanylurea phosphate, Melamine Cyanurate (MCA), melamine phosphate, melamine pyrophosphate, chloro ester resin, chloro-partial resin, brominated styrene, brominated epoxy resin, polyvinyl chloride, chlorinated paraffin, methyl chloride, cyclic phosphate ester, tris (1, 3-dichloroisopropyl) phosphate (TDCPP), tris (2-chloropropyl) phosphate (TCPP), tris (2-chloroethyl) phosphate (TCEP), triisopropylphenyl phosphate (IPPP), triisobutyl phosphate (TIBP), One or more of tricresyl phosphate (TCP), diphenylisodecyl phosphate (DPDP), diphenylisooctyl phosphate (DPOP), triethyl phosphate (TEP), trimethyl phosphate (TMP), trixylyl phosphate (TXP), cresyldiphenyl phosphate (CDP), triphenyl phosphate (TPP), tris (butoxyethyl) phosphate (TBEP; TBXP; KP-140), resorcinol-bis (diphenyl phosphate (RDP), bisphenol A-bis (diphenyl phosphate) (BDP), resorcinol bis [ bis (2, 6-dimethylphenyl) phosphate ] (RDX), polyaryl phosphate (PX-220), 9, 10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide (DOPO), aluminum hydroxide, magnesium hydroxide, and talc flame retardants.
Preferably, the polyvinyl alcohol in the first step comprises one or more of polyvinyl alcohol with a polymerization degree of 50-2600 and a alcoholysis degree of 50% -99%.
Preferably, the auxiliary agent in the first step comprises one or more of boric acid, borax, aziridine, melamine formaldehyde resin, an adduct of isocyanate and trimethylolpropane, blocked isocyanate, a thickening agent, a dispersing agent, an emulsifying agent, a PH adjusting agent, a bactericide and a defoaming agent.
The beneficial effects of the invention are as follows:
1. antimony trioxide is not used, so that adverse effects of heavy metals such as lead, arsenic and cadmium contained in the antimony trioxide on human health are avoided.
2. Through setting up polyvinyl alcohol as the carbon former, the char formation nature is good when the fabric burns, has splendid resistant burn-through nature good, and when the fabric burns, there is not the drippage to produce, has avoided drippage not have the drippage to ignite other combustible substance, has also effectively avoided, still has better resistant burn-through nature after the water logging.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the embodiments of the present invention, 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.
A preparation method of antimony-free burn-through-resistant water-based flame retardant adhesive for a fabric coating comprises the following steps of preparing raw materials in parts by weight:
the total weight of the raw materials is 100 parts;
in the first step, the aqueous resin comprises one or more of ethylene-vinyl acetate copolymer emulsion, acrylate emulsion, polyurethane emulsion, butylbenzene emulsion and butyronitrile emulsion, and the solid content of the aqueous resin is 20-60%;
the flame retardant in the first step comprises Hexabromocyclododecane (HBCD), decabromodiphenyl ether, decabromodiphenylethane, tris (2, 3-dibromopropyl) isocyanurate, bromotriazine, ethylenebistetrabromophthalimide, tetrabromobisphenol A, octabromoether, methyl octabromoether, ammonium polyphosphate (APP), guanidine phosphate, guanylurea phosphate, Melamine Cyanurate (MCA), melamine phosphate, melamine pyrophosphate, chloro ester resin, chloro-meta-resin, brominated styrene, brominated epoxy resin, polyvinyl chloride, chlorinated paraffin, methyl chloride, cyclic phosphate ester, tris (1, 3-dichloroisopropyl) phosphate (TDCPP), tris (2-chloropropyl) phosphate (TCPP), tris (2-chloroethyl) phosphate (TCEP), triisopropylphenyl phosphate (IPPP), triisobutyl phosphate (TIBP), One or more of tricresyl phosphate (TCP), diphenylisodecyl phosphate (DPDP), diphenylisooctyl phosphate (DPOP), triethyl phosphate (TEP), trimethyl phosphate (TMP), trixylyl phosphate (TXP), cresyldiphenyl phosphate (CDP), triphenyl phosphate (TPP), tris (butoxyethyl) phosphate (TBEP; TBXP; KP-140), resorcinol-bis (diphenyl phosphate (RDP), bisphenol A-bis (diphenyl phosphate) (BDP), resorcinol bis [ bis (2, 6-dimethylphenyl) phosphate ] (RDX), polyaryl phosphate (PX-220), 9, 10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide (DOPO), aluminum hydroxide, magnesium hydroxide, and talc flame retardants;
in the first step, polyvinyl alcohol comprises one or more of polyvinyl alcohol with the polymerization degree of 50-2600% and the alcoholysis degree of 50% -99%;
the auxiliary agent in the first step comprises one or more of boric acid, borax, aziridine, melamine formaldehyde resin, an addition product of isocyanate and trimethylolpropane, blocked isocyanate, a thickening agent, a dispersing agent, an emulsifying agent, a pH regulator, a bactericide and a defoaming agent;
preparing a finished product by the processes of preparing a solution of polyvinyl alcohol, preparing a powder flame retardant aqueous dispersion, pretreating a phosphate flame retardant, mixing and filtering;
step two, preparing a polyvinyl alcohol solution,
adding the polyvinyl alcohol obtained in the step one into a container with a stirring and heating device, adding water with the weight 2-8 times that of the polyvinyl alcohol, slowly stirring until the polyvinyl alcohol is fully dissolved, starting the heating device when the polyvinyl alcohol which is not easily dissolved at normal temperature is used, raising the temperature to 50-95 ℃, continuously stirring until the polyvinyl alcohol is fully dissolved, then adding the cross-linking agent, the bactericide and the defoaming agent in the auxiliary agent obtained in the step one, and stirring to obtain a polyvinyl alcohol aqueous solution for later use;
step three, preparing the powder flame retardant water dispersion liquid,
adding the balance of the water in the step one and the dispersing agent and the wetting agent in the auxiliary in the step one into a container with a stirring device, and stirring for 1-5 minutes; then adding the powder flame retardant while stirring, increasing the stirring speed to more than 1000 revolutions per minute, continuing stirring, and filtering for later use after the powder flame retardant is fully dispersed in water;
step four, pre-treating the phosphate flame retardant,
adding one or more phosphate flame retardants in the step one into a container with a stirring and heating device, starting the stirring device, and stirring; after stirring at normal temperature, if solid phosphate flame retardant exists, starting the heating device, and continuing stirring to enable the system to be in a liquid state. Removing impurities to prepare the liquid phosphate flame retardant for later use.
Step five, preparing the flame-retardant adhesive,
adding the rest of water, the water-based resin and the polyvinyl alcohol solution prepared in the step two into a container with a stirring device, adding the powdery flame retardant aqueous dispersion prepared in the step three, starting a stirrer, slowly stirring for 1-10 minutes, adding the phosphate flame retardant pretreated in the step four, increasing the rotating speed of the stirrer to be more than 1000 revolutions per minute, stirring until the mixture is fully and uniformly mixed, checking the viscosity condition of the mixture, adding a thickening agent to increase the consistency, preparing a finished product, discharging and packaging.
By arranging the polyvinyl alcohol as the carbonizing agent, the fabric has good carbonizing property during combustion, excellent burn-through resistance, no dripping substance is generated during the combustion of the fabric, other inflammable substances are prevented from being ignited by dripping and no dripping substance, and the fabric still has good burn-through resistance after being soaked in water;
antimony trioxide is not used, so that the adverse effect of heavy metal contained in the antimony trioxide on the health of a human body is avoided.
Example one
A method for preparing antimony-free water-based flame retardant adhesive for a fabric coating,
step one, preparing raw materials, which comprises the following components in parts by weight:
the total weight of the raw materials is 100 parts
Step two, preparing a polyvinyl alcohol solution,
adding 6 parts of polyvinyl alcohol and 30 parts of water into a container with a stirring device and a heating device, starting a stirrer, stirring at a low speed for 1-4 hours, starting the heating device, raising the temperature to 50-95 ℃, and continuing stirring for 2 hours to fully dissolve the polyvinyl alcohol. Continuously stirring at a low speed, adding a bactericide, a defoaming agent and a crosslinking agent to prepare a polyvinyl alcohol aqueous solution, and discharging for later use;
step three, preparing the powder flame retardant water dispersion liquid,
adding 10 parts of water into a container with a stirring device, adding the dispersing agent and the wetting agent in the auxiliary agent in the step one, starting the stirring device, stirring for 1-5 minutes, adding the decabromodiphenylethane and the ammonium polyphosphate in the step one, stirring for 10-20 minutes, preparing a powdery flame retardant aqueous dispersion after the decabromodiphenylethane and the ammonium polyphosphate are fully dispersed, filtering, and discharging for later use;
step four, pre-treating the phosphate flame retardant,
adding TDCPP into a container with stirring and heating functions, and starting a stirring device. After stirring at normal temperature, if solid phosphate flame retardant exists, starting the heating device, and continuing stirring to enable the system to be in a liquid state. Removing impurities to prepare a liquid phosphate flame retardant for later use;
step five, preparing the flame-retardant adhesive,
and (3) adding the aqueous resin in the step one into a container with a stirring device, starting the stirring device, stirring at a low speed, adding the polyvinyl alcohol solution in the step two, adding the flame retardant dispersion liquid in the step three, adding the liquid TDCPP pretreated in the step four, regulating the stirring speed to 1000-3000 r/min, after fully mixing, adding the thickening agent according to the viscosity, discharging and packaging.
Example two
A preparation method of antimony-free water-based flame retardant adhesive for fabric coating comprises the following steps of preparing raw materials in parts by weight:
step two, preparing a polyvinyl alcohol solution,
and (3) adding the polyvinyl alcohol (PVA 2488) obtained in the step one into a container with a stirring device and a heating device, adding 30 parts of water, starting a stirrer, and slowly stirring for 1-4 hours. And (3) starting a heating device, heating to 80-95 ℃, continuing to stir for 2 hours to fully dissolve the polyvinyl alcohol, adding the cross-linking agent, the bactericide and the defoaming agent in the auxiliary in the step one, and continuing to stir for 10-30 minutes. Preparing a polyvinyl alcohol aqueous solution for later use;
step three, preparing the powder flame retardant water dispersion liquid,
adding 15 parts of water in the first step into the dispersing agent and the wetting agent in the auxiliary agent in the first step in a container with a stirring device, stirring for 1-5 minutes, adding decabromodiphenylethane and ammonium polyphosphate, stirring for 10-20 minutes, directly and completely dispersing the decabromodiphenylethane and the ammonium polyphosphate, and filtering to prepare a powder flame retardant aqueous dispersion for later use;
step four, pre-treating the phosphate flame retardant,
adding a fire retardant PX 220 and TDCPP into a container with a stirring and stirring device and a heating device, starting the heating and stirring device, removing impurities after the fire retardant PX 220 and TDCPP are completely in a liquid state, and discharging for later use;
step five, preparing the flame-retardant glue,
and (3) adding the aqueous resin obtained in the step one into a stirrer, starting the stirrer, stirring at a low speed, adding the polyvinyl alcohol solution obtained in the step two, the powdery flame retardant water dispersion obtained in the step three, regulating the stirring speed of the liquid phosphate flame retardant obtained in the step four to 1000-3000 r/min, after fully mixing, adding a thickener according to the viscosity, discharging and packaging.
EXAMPLE III
A preparation method of antimony-free water-based flame retardant adhesive for fabric coating comprises the following steps of preparing raw materials in parts by weight:
the weight of the raw materials is 100 parts in total
Step two, preparing a polyvinyl alcohol solution,
and (3) adding the polyvinyl alcohol (PVA 1799) in the step one into a container with a stirring device and a heating device, adding water which is 3-6 times of the polyvinyl alcohol, starting a stirrer, and slowly stirring for 1-4 hours. And (3) starting a heating device, heating to 80-95 ℃, continuing to stir for 2 hours to fully dissolve the polyvinyl alcohol, adding the cross-linking agent and the bactericide in the auxiliary in the step one, and continuing to stir for 10-30 minutes. Preparing polyvinyl alcohol solution for later use;
step three, preparing the powder flame retardant water dispersion liquid,
adding the balance of water in the step one into a container with a stirring device, adding a dispersing agent and a wetting agent in the auxiliary agent in the step one, stirring for 1-5 minutes, then adding ammonium polyphosphate, stirring for 10-20 minutes, directly and completely dispersing the ammonium polyphosphate, filtering, and discharging for later use;
step four, pre-treating the phosphate flame retardant,
adding flame retardant TPP and TDCPP into a container with a stirring and stirring device and a heating device, starting the heating and stirring device, removing impurities after the mixture is completely in a liquid state, and discharging for later use;
step five, preparing the flame-retardant adhesive,
and (3) adding the waterborne resin obtained in the step one into a stirrer, starting the stirrer, stirring at a low speed, adding the polyvinyl alcohol solution obtained in the step two, adding the ammonium polyphosphate water dispersion obtained in the step three, adding the liquid phosphate fire retardant obtained in the step four, regulating the stirring speed to 1000-3000 r/min, adding a thickening agent according to the viscosity after fully mixing, and finally filtering, discharging and packaging.
Example four
A preparation method of antimony-free water-based flame retardant adhesive for fabric coating comprises the following steps of preparing raw materials in parts by weight:
step two, preparing a polyvinyl alcohol solution,
and (3) adding the polyvinyl alcohol (PVA 1799) in the step one into a container with a stirring device and a heating device, adding water which is 3-6 times of the polyvinyl alcohol, starting a stirrer, and slowly stirring for 1-4 hours. And (3) starting a heating device, heating to 80-95 ℃, continuing to stir for 2 hours to fully dissolve the polyvinyl alcohol, adding the cross-linking agent, the bactericide and the defoaming agent in the auxiliary in the step one, and continuing to stir for 10-30 minutes. Standby;
step three, preparing the aqueous dispersion of the powdery flame retardant,
adding the water in the first step into the dispersant and the wetting agent in the auxiliary in the first step in a container with a stirring device, stirring for 1-5 minutes, then adding decabromodiphenylethane and ammonium polyphosphate, stirring for 10-20 minutes until the decabromodiphenylethane and the ammonium polyphosphate are completely dispersed, filtering, and discharging for later use;
step four, pretreatment of the phosphate flame retardant.
Adding flame retardant TPP and TDCPP into a container with a stirring and stirring device and a heating device, starting the heating and stirring device, removing impurities after the mixture is completely in a liquid state, and discharging for later use;
step five, preparing the flame-retardant adhesive,
and (3) adding the aqueous resin in the step one into a stirrer, starting the stirrer, stirring at a low speed, adding the polyvinyl alcohol solution prepared in the step two, adding the aqueous dispersion of decabromodiphenylethane and ammonium polyphosphate prepared in the step three, adding the liquid phosphate flame retardant prepared in the step four, regulating the stirring speed to 1000-3000 r/min, after fully mixing, adding a thickener according to viscosity, discharging and packaging.
EXAMPLE five
A preparation method of antimony-free water-based flame retardant adhesive for fabric coating comprises the following steps of preparing raw materials in parts by weight:
the total weight of the raw materials is 100 parts;
step two, preparing a polyvinyl alcohol solution,
and (3) adding the polyvinyl alcohol (PVA 1799) in the step one into a container with a stirring device and a heating device, adding all the water in the step one, starting a stirrer, and slowly stirring for 1-4 hours. And (3) starting a heating device, heating to 80-95 ℃, continuing to stir for 2 hours to fully dissolve the polyvinyl alcohol, adding the cross-linking agent, the bactericide and the defoaming agent in the auxiliary in the step one, and continuing to stir for 10-30 minutes. Preparing a polyvinyl alcohol aqueous solution for later use;
step three, pre-treating the phosphate flame retardant,
adding fire retardants RDP, TPP and TDCPP into a container with a stirring and stirring device and a heating device, starting the heating and stirring device, and removing impurities after the mixture is completely liquid to prepare the liquid phosphate fire retardant. Standby;
step four, the preparation of the flame-retardant adhesive,
adding water-based resin into the mixture with a stirring device, starting the stirring device, stirring at a low speed, adding the polyvinyl alcohol solution prepared in the step two, regulating the stirring speed of the liquid phosphate fire retardant prepared in the step three to 3000 revolutions per minute, adding a thickening agent according to the viscosity after fully mixing, discharging and packaging.
EXAMPLE six
A preparation method of antimony-free water-based flame retardant adhesive for fabric coating comprises the following steps of preparing raw materials in parts by weight:
step two, preparing a polyvinyl alcohol solution,
and (3) adding the polyvinyl alcohol obtained in the step one into a container with a stirring and heating device, adding water which is 2-5 times of the polyvinyl alcohol, stirring at a low speed, starting the heating device, raising the temperature to 50-95 ℃, and continuing stirring until the polyvinyl alcohol is fully dissolved. Then, adding the cross-linking agent, the bactericide and the defoaming agent in the auxiliary agent in the step one, and stirring to prepare a polyvinyl alcohol aqueous solution for later use;
step three, preparing the powder flame retardant water dispersion liquid,
adding the balance of the water in the step one and the dispersing agent and the wetting agent in the auxiliary in the step one into a container with a stirring device, and stirring for 1-5 minutes; then adding ammonium polyphosphate fire retardant while stirring, increasing the stirring speed to more than 1000 r/min, continuing stirring, and filtering after the fire retardant is fully dispersed in water. Preparing the powdery flame retardant water dispersion for later use.
Step four, pretreatment of the phosphate flame retardant
And (3) adding the TDCPP and TCPP starting stirring devices in the step I into a container with a stirring and heating device, and stirring. After stirring at normal temperature, if solid phosphate flame retardant exists, starting the heating device, and continuing stirring to enable the system to be in a liquid state. Removing impurities to prepare a liquid phosphate flame retardant for later use;
step five, preparing the flame-retardant adhesive,
and (3) adding the water-based resin, the polyvinyl alcohol solution prepared in the step two, the aqueous dispersion of the powdery flame retardant prepared in the step three and the liquid phosphate flame retardant pretreated in the step four into a container with a stirring device, increasing the rotating speed of the stirrer to be more than 1000 rpm, and stirring until the mixture is fully and uniformly mixed. Checking viscosity, adding thickener to increase consistency if necessary, making into final product, discharging, and packaging.
EXAMPLE seven
A method for preparing antimony-free water-based flame retardant adhesive for a fabric coating, which comprises the following steps of preparing raw materials,
comprises the following components in parts by weight:
step two, preparing a polyvinyl alcohol solution,
and (2) adding the polyvinyl alcohol obtained in the step one into a container with a stirring and heating device, adding water which is 2-6 times of the polyvinyl alcohol, stirring at a low speed, starting the heating device, raising the temperature to 50-95 ℃, continuing stirring until the polyvinyl alcohol is fully dissolved, then adding the cross-linking agent, the bactericide and the defoaming agent in the auxiliary agent obtained in the step one, and stirring to obtain a polyvinyl alcohol aqueous solution for later use.
Step three, preparing the powder flame retardant water dispersion liquid,
adding the balance of the water in the step one and the dispersing agent and the wetting agent in the auxiliary in the step one into a container with a stirring device, and stirring for 1-5 minutes; then adding ammonium polyphosphate fire retardant while stirring, increasing the stirring speed to more than 1000 r/min, continuing stirring, and filtering for later use after the fire retardant is fully dispersed in water.
And step four, pretreating the phosphate flame retardant.
And (3) adding a TDCPP and TCP starting stirring device into a container with a stirring and heating device, and stirring. After stirring at normal temperature, if solid phosphate flame retardant exists, starting the heating device, and continuing stirring to enable the system to be in a liquid state. Removing impurities to prepare the liquid phosphate flame retardant for later use.
Step five, preparing the flame-retardant adhesive,
and (3) adding the water-based resin and the polyvinyl alcohol solution prepared in the step two into a container with a stirring device, adding the ammonium polyphosphate water dispersion prepared in the step three, starting a stirrer, stirring at a low speed for 1-10 minutes, adding the pretreated TDCPP and TCPP flame retardant prepared in the step four, increasing the rotating speed of the stirrer to be more than 1000 revolutions per minute, and stirring until the materials are fully and uniformly mixed. Checking viscosity, adding thickener to increase consistency if necessary, making into final product, discharging, and packaging.
The above description is only for the preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art should be considered to be within the technical scope of the present invention, and the technical solutions and the inventive concepts thereof according to the present invention should be equivalent or changed within the scope of the present invention.
Claims (5)
1. A preparation method of antimony-free burn-through resistant water-based flame retardant adhesive for fabric coating is characterized by comprising the following steps: step one, preparing raw materials, which comprises the following components in parts by weight:
the total weight of the raw materials is 100 parts;
step two, preparing a polyvinyl alcohol solution,
adding the polyvinyl alcohol obtained in the step one into a container with a stirring and heating device, adding water with the weight 2-8 times that of the polyvinyl alcohol, slowly stirring until the polyvinyl alcohol is fully dissolved, starting the heating device when the polyvinyl alcohol which is not easily dissolved at normal temperature is used, raising the temperature to 50-95 ℃, continuously stirring until the polyvinyl alcohol is fully dissolved, then adding the cross-linking agent, the bactericide and the defoaming agent in the auxiliary agent obtained in the step one, and stirring to obtain a polyvinyl alcohol aqueous solution for later use;
step three, preparing the powder flame retardant water dispersion liquid,
adding the balance of the water in the step one and the dispersing agent and the wetting agent in the auxiliary in the step one into a container with a stirring device, and stirring for 1-5 minutes; then adding the powder flame retardant while stirring, increasing the stirring speed to more than 1000 revolutions per minute, continuing stirring, fully dispersing the powder flame retardant in water, and filtering to obtain a powder flame retardant aqueous dispersion for later use;
step four, pre-treating the phosphate flame retardant,
adding one or more phosphate flame retardants in the step one into a container with a stirring and heating device, starting the stirring device, and stirring; after stirring at normal temperature, starting a heating device and continuing stirring to enable the system to be in a liquid state, removing impurities and preparing a liquid phosphate flame retardant for later use;
step five, preparing the flame-retardant adhesive,
adding the water-based resin obtained in the step one into a container with a stirring device, adding the polyvinyl alcohol solution obtained in the step two, adding the powdery flame retardant aqueous dispersion obtained in the step three, starting a stirrer, slowly stirring for 1-10 minutes, adding the liquid phosphate flame retardant pretreated in the step four, increasing the rotating speed of the stirrer to be more than 1000 revolutions per minute, stirring until the mixture is fully and uniformly mixed, checking the viscosity condition of the mixture, and adding a thickening agent to increase the consistency; and (5) preparing a finished product, discharging and packaging.
2. The preparation method of the antimony-free burn-through resistant water-based flame retardant adhesive for the fabric coating according to claim 1 is characterized in that: the aqueous resin in the first step comprises one or more of ethylene-vinyl acetate copolymer emulsion, acrylate emulsion, polyurethane emulsion, butylbenzene emulsion and butyronitrile emulsion, and the solid content of the aqueous resin is 20% -60%.
3. The preparation method of the antimony-free burn-through resistant water-based flame retardant adhesive for the fabric coating according to claim 1 is characterized in that: the flame retardant in the first step comprises Hexabromocyclododecane (HBCD), decabromodiphenyl ether, decabromodiphenylethane, tris (2, 3-dibromopropyl) isocyanurate, bromotriazine, ethylenebistetrabromophthalimide, tetrabromobisphenol A, octabromoether, methyl octabromoether, ammonium polyphosphate (APP), guanidine phosphate, guanylurea phosphate, Melamine Cyanurate (MCA), melamine phosphate, melamine pyrophosphate, chloro ester resin, chloro-partial resin, brominated styrene, brominated epoxy resin, polyvinyl chloride, chlorinated paraffin, methyl chloride, cyclic phosphate ester, tris (1, 3-dichloroisopropyl) phosphate (TDCPP), tris (2-chloropropyl) phosphate (TCPP), tris (2-chloroethyl) phosphate (TCEP), triisopropylphenyl phosphate (IPPP), triisobutyl phosphate (TIBP), One or more of tricresyl phosphate (TCP), diphenylisodecyl phosphate (DPDP), diphenylisooctyl phosphate (DPOP), triethyl phosphate (TEP), trimethyl phosphate (TMP), trixylyl phosphate (TXP), cresyldiphenyl phosphate (CDP), triphenyl phosphate (TPP), tris (butoxyethyl) phosphate (TBEP; TBXP; KP-140), resorcinol-bis (diphenyl phosphate (RDP), bisphenol A-bis (diphenyl phosphate) (BDP), resorcinol bis [ bis (2, 6-dimethylphenyl) phosphate ] (RDX), polyaryl phosphate (PX-220), 9, 10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide (DOPO), aluminum hydroxide, magnesium hydroxide, and talc flame retardants.
4. The preparation method of the antimony-free burn-through resistant water-based flame retardant adhesive for the fabric coating according to claim 1 is characterized in that: in the first step, the polyvinyl alcohol comprises one or more of polyvinyl alcohol with the polymerization degree of 50-2600 and the alcoholysis degree of 50-99%.
5. The preparation method of the antimony-free burn-through resistant water-based flame retardant adhesive for the fabric coating according to claim 1 is characterized in that: the auxiliary agent in the first step comprises one or more of boric acid, borax, aziridine, melamine formaldehyde resin, an addition product of isocyanate and trimethylolpropane, blocked isocyanate, a thickening agent, a dispersing agent, an emulsifying agent, a pH regulator, a bactericide and a defoaming agent.
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Application publication date: 20191231 |