CN111748231A - Synthesis method of antimony oxide sol and flame-retardant auxiliary - Google Patents

Synthesis method of antimony oxide sol and flame-retardant auxiliary Download PDF

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CN111748231A
CN111748231A CN202010595627.1A CN202010595627A CN111748231A CN 111748231 A CN111748231 A CN 111748231A CN 202010595627 A CN202010595627 A CN 202010595627A CN 111748231 A CN111748231 A CN 111748231A
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sol
water
halogen
gamma
antimony
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不公告发明人
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Sichuan Sidi New Material Co ltd
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Sichuan Sidi New Material Co ltd
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    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
    • C09D5/00—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
    • C09D5/18—Fireproof paints including high temperature resistant paints
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
    • C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
    • C09D7/40—Additives
    • C09D7/60—Additives non-macromolecular
    • C09D7/63—Additives non-macromolecular organic
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
    • C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
    • C09D7/40—Additives
    • C09D7/65—Additives macromolecular

Abstract

The invention discloses a synthesis method of antimony oxide sol and a flame-retardant auxiliary agent. The method comprises the following steps: (1) uniformly dispersing water, a sol stabilizer, antimony trioxide, a modifier and the like, dropwise adding hydrogen peroxide, and heating the mixture to 70-95 ℃ to obtain a mixture of antimony oxides in a sol state; (2) adding a pH regulator, and adding one or two of molybdenum trioxide sol or molybdenum disulfide sol; (3) concentrating to the required concentration. The sol prepared by the invention is stable, transparent and micro-emulsion white. The material prepared by the method is a flame retardant auxiliary agent with excellent performance in the field of water-based paint.

Description

Synthesis method of antimony oxide sol and flame-retardant auxiliary
Technical Field
The invention relates to a method for synthesizing antimony oxide sol and a flame-retardant auxiliary agent, and the product is particularly suitable for application of a water-based paint system.
Background
China is the most abundant country in the world with antimony ore. The nationwide reserve of antimony accounts for 51.8% of the world's total reserves. Although the supply amount of antimony products accounts for nearly half of the world, the deep processing rate of antimony products in China is low, antimony trioxide is the most important product consuming antimony resources in China, the using amount of the antimony trioxide reaches more than 80%, and 60% of antimony is used for producing the flame retardant antimony trioxide, so that the saving and application of the non-renewable antimony resources are of great significance. At present, the high-efficiency flame retardance of a bromine-antimony flame retardant system still has wide application in the flame retardant industry, so that the consumption of low-efficiency antimony materials in China is reduced, and the effective application of the antimony materials is urgent.
Antimony trioxide and hydrogen peroxide (H)2O2) Under the condition of heating, the nano antimony pentoxide sol can be easily prepared, and because the antimony pentoxide is dispersed in water solution in nano level and the grain size is less than 20 nm, the antimony pentoxide sol has a large chemical reaction interface and can be more quickly preparedChemical response improves the synergistic flame retardance to the organic bromine. The molar ratio of the antimony trioxide to the hydrogen peroxide is more than or equal to 1: 2, hydrogen peroxide is liable to remain in the reaction system, and this causes unnecessary damage to the aqueous coating system.
CN 101941737A discloses mixing antimony trioxide, hydrogen peroxide, deionized water and an inert porous material, filtering and drying a product after the reaction is finished, and obtaining a white antimony pentoxide solid with a core-shell structure. For a water-based paint system, the powder with the core-shell structure is easy to agglomerate and difficult to disperse, and the interface of antimony oxide is easy to reduce, namely the synergistic flame retardance of antimony pentoxide is reduced.
CN 108793250A discloses a synthesis method for preparing antimony pentoxide by adding hydrogen peroxide dropwise after heating, wherein the molar ratio of antimony trioxide to hydrogen peroxide is 2.0-2.5, and stabilizer triethanolamine is added more than or equal to 4 times. The aqueous solution prepared by the method has low concentration, and the existence of excessive hydrogen peroxide has great destructiveness to the stability of the coating for a water-based coating system, so that the aqueous solution can not be applied to a steel structure flame-retardant coating.
CN 104828866A discloses a preparation method of colloidal antimony oxide dry powder with low volatility at high temperature. And adding metal hydroxide (sodium hydroxide and/or potassium hydroxide) into the prepared antimony pentoxide solution to adjust the pH value, and adding a reducing agent for partial reduction to obtain antimony oxide sol. Removing alkali metal ions in the antimony oxide sol by ion exchange. The method has the advantages of complex process flow, high energy consumption and solid waste generation.
CN 106366723A discloses a burn-through resistant water-based flame retardant adhesive for textile, which comprises a water-based adhesive, a water-based flame retardant adhesive, a halogen flame retardant, a synergistic flame retardant, an auxiliary agent and water. Wherein the water-based adhesive comprises ethylene-vinyl acetate copolymer emulsion and auxiliary adhesive; the water-based flame-retardant gum phosphate flame retardant comprises one or more of ammonium polyphosphate, ammonium phosphate, guanidine phosphate, guanylurea phosphate, melamine phosphate and melamine pyrophosphate, or one or more of alkyl phosphate, condensed phosphate, phenyl phosphate, cage-shaped and spiro-shaped phosphate and cyclic phosphate. The halogen flame retardant comprises one or more of decabromodiphenyl ether, decabromodiphenyl ethane, brominated epoxy resin, polyvinyl chloride, chlorinated paraffin, methyl chloride and the like; the inorganic flame retardant comprises one or more of antimony trioxide, zinc borate, zinc oxide, aluminum hydroxide, arsenic trioxide, antimony pentoxide, magnesium hydroxide, vermiculite powder, talcum powder, calcium carbonate, titanium dioxide, montmorillonite, kaolin, barium sulfate, mica powder, fluorite powder, glass micropowder, expanded graphite, a molecular sieve and zeolite. In order to improve the good dispersibility of the particles, the method needs to break the particles in the liquid by grinding equipment, and the obtained liquid contains micron-sized solid particles, so that the application of the method has certain limitation for thin coatings.
CN 1550453a discloses a method for synthesizing antimony pentoxide by doping molybdate or tungstate, which must use soluble molybdate or tungstate to effectively dope antimony pentoxide.
Disclosure of Invention
The water-based thin coating system has strict requirements on the filler type flame retardant, such as the particle size and the addition amount of the filler. Improper addition can result in poor adhesion of the coating to the substrate and the coating is prone to cracking. The bromine antimony flame retardant has the advantages of small addition amount in the coating, high flame retardant efficiency and small influence on the coating, and is a very effective flame retardant auxiliary agent. However, antimony trioxide used in the industry is white powder with the particle size of about 1-5 microns, and is white suspension in an aqueous system, so that the coating is easy to delaminate, a film-forming substance is easy to crack, and the antimony trioxide cannot be applied to a transparent coating, so that the development and enrichment of antimony pentoxide flame retardant additives are necessary. Aiming at the problems, the invention provides a stable and transparent water-based flame retardant additive, which takes water-based resin and inorganic salt as stabilizers and has good intermiscibility and good film forming property in water-based paint. The paint prepared by the material realizes good flame retardance, strong coating adhesion and difficult cracking, and can also be applied to the field of transparent flame retardant coatings.
The technical scheme adopted by the invention for solving the technical problems is as follows: the synthesis of antimony oxide sol and the preparation of flame retardant additive comprise the following steps:
(1) uniformly dispersing water, a sol stabilizer, antimony trioxide, a modifier and the like, dropwise adding hydrogen peroxide, and heating the mixture to 70-95 ℃ to obtain a mixture of antimony oxides in a sol state;
(2) adding a pH regulator, and adding one or two of molybdenum trioxide sol and molybdenum disulfide sol;
(3) concentrating to the required concentration.
According to the claims: uniformly dispersing water, a sol stabilizer, antimony trioxide, a modifier and the like, dropwise adding hydrogen peroxide, and heating the mixture to 70-95 ℃ to obtain a mixture of antimony oxides in a sol state.
The sol stabilizer is one or more of bisulfate and organic resin, and the bisulfate is preferably sodium bisulfate. The organic resin can be dispersed in water, and comprises one or more of water-based halogen-free or halogen-containing saturated polyester, water-based halogen-free or halogen-containing unsaturated polyester, water-based halogen-free or halogen-containing polyurethane, water-based halogen-free or halogen-containing epoxy resin, water-based halogen-free or halogen-containing acrylic resin, water-based halogen-free or halogen-containing polyolefin resin, polyethylene glycol, polyvinylpyrrolidone, polyethylene oxide, polylactic acid and polyvinyl alcohol.
The resin is capable of aqueous dispersion and has the following characteristics: the resin is soluble in water or a mixed solvent of water and alcohol; or the resin can be dissolved in an organic solvent, and the resulting solution can be dispersed in water with added surfactant to form a water-soluble emulsion. The resin comprises and not only comprises one or more of aqueous halogen-free or halogen-containing saturated polyester, aqueous halogen-free or halogen-containing unsaturated polyester, aqueous halogen-free or halogen-containing polyurethane, aqueous halogen-free or halogen-containing epoxy resin, aqueous halogen-free or halogen-containing acrylic resin, aqueous halogen-free or halogen-containing olefin resin, polyethylene glycol, polyvinylpyrrolidone, polylactic acid and polyvinyl alcohol. Preferably waterborne polyurethane or waterborne epoxy resin, and the weight ratio of the mass of the bromine element to the total mass of the resin is not less than 5 percent.
The molecular weight and alcoholysis degree of the polyvinyl alcohol and resin have great influence on the hydrolyzability and the film forming property, and the grade 1799 is preferred. The aqueous halogen-free or halogen-containing polyester is preferably a low molecular weight water-soluble polyester. The aqueous halogen-free or halogen-containing polyurethane is preferably aqueous polyurethane resin containing bromine. The water-based halogen-free or halogen-containing acrylic resin is preferably an organosilicon modified acrylic resin. The aqueous halogen-free or halogen-containing olefin resin is preferably polyethylene-vinyl acetate copolymer.
The hydrogen peroxide is liquid containing hydrogen peroxide with the concentration of 25-50%, and the concentration of 30% is preferred.
The modifier is a silane coupling agent and comprises one or more of tetramethoxysilane, phenyltrimethoxysilane, phenyltriethoxysilane, tetraethoxysilane, methyltrimethoxysilane, ethyltrimethoxysilane, ethyltriethoxysilane, propyltrimethoxysilane, dimethyldimethoxysilane, gamma-aminopropyltriethoxysilane, gamma-aminopropyltrimethoxysilane, gamma- (2, 3-epoxypropoxy) propyltrimethoxysilane, gamma-methacryloxypropyltrimethoxysilane, N- (beta-aminoethyl) -gamma-aminopropyltriethoxysilane, N-beta- (aminoethyl) -gamma-aminopropyltrimethoxysilane, N-beta- (aminoethyl) -gamma-aminopropylmethyldimethoxysilane, N-beta- (aminoethyl) -gamma-aminopropyl-trimethoxysilane, and/or a mixture thereof, One or more of gamma-aminopropylmethyldimethoxysilane, gamma-aminopropylmethyldiethoxysilane, vinyltriethoxysilane, vinyltrimethoxysilane, vinyltris (beta-methoxyethoxy) silane, silica powder or silica sol; gamma-aminopropyltriethoxysilane, gamma-methacryloxypropyltrimethoxysilane, gamma- (2, 3-glycidoxy) propyltrimethoxysilane are preferred. Preferably, the mixture of tetramethoxysilane, methyltrimethoxysilane and gamma- (2, 3-epoxypropoxy) propyl trimethoxysilane, silicon dioxide powder or silicon dioxide sol is prepared from the following components in a mass ratio of 2: 2: 1.
the molybdenum trioxide sol and the molybdenum disulfide sol refer to a nano aqueous dispersion of molybdenum trioxide or molybdenum disulfide, and the molybdenum trioxide sol is characterized in that the particle size of molybdenum trioxide is less than 200 nanometers, the solid content of the molybdenum trioxide sol is less than or equal to 45 percent, the molybdenum trioxide sol is a colorless transparent liquid, and the shape of the nano particles is spherical. The molybdenum disulfide is a flake nano dispersion liquid, the flake diameter is less than 200 nanometers, and the flake thickness is less than 50 nanometers. Molybdenum trioxide sols are preferred.
The mass ratio of the water to the stabilizer to the antimony trioxide to the silane coupling agent is 3-8: 0.05-0.2: 1: 0.02 to 0.15. Wherein the mass ratio of the sodium bisulfate to the solid content of the water-based resin is 1: 0.1 to 10. In the preparation process, sodium bisulfate needs to be dissolved to 10-18 percent, a high-concentration solution is not suitable, otherwise, the solution obtained in the step (1) is milky turbid. The aqueous resin addition time was complete before the addition of the sodium bisulfate solution. Before adding, the pH value of the aqueous resin needs to be tested and adjusted to be 5-8, the pH value of an acidic aqueous resin solution does not need to be regulated, and an organic or inorganic acid aqueous solution needs to be used for adjusting an alkaline aqueous resin solution to be 5-8.
The molar ratio of the hydrogen peroxide to the antimony trioxide in the hydrogen peroxide is less than 2, preferably 1.60-1.99. Excessive hydrogen peroxide can cause hydrogen peroxide residue in reaction products, and the residual hydrogen peroxide can affect the preparation of the water-based paint and cause the occurrence of poor coating.
The pH regulator comprises an alkali metal or alkaline earth metal hydroxide, preferably sodium hydroxide or potassium hydroxide, or a mixture thereof.
One or two of the molybdenum trioxide sol and the molybdenum disulfide sol. The mass ratio of the total mass of the solids contained in the molybdenum trioxide or molybdenum disulfide sol to the total mass of the solids of the antimony oxide sol prepared in the step (1) is 0.05-0.2, and the preferred mass ratio is 0.1.
And (3) concentrating the liquid in the step (3), wherein the concentration temperature is 75-105 ℃. Distillation under atmospheric or reduced pressure, preferably reduced pressure.
The flame-retardant auxiliary agent prepared by the invention has the following characteristics:
the product is a transparent white aqueous solution, is easy to add into a water-based paint, can be added in a large amount, has excellent flame retardant property, and reduces the harm to the environment due to the smoke suppressant. The product has excellent stability, can be stored and transported for a long time, and the obtained coating does not crack, has flat and smooth surface and crystal-clear and transparent appearance. The solution contains particles with the particle size less than 200 nanometers, so the solution has strong permeability to base materials and good permeability to wood or artificial boards, and the product is particularly suitable for floor flame retardance.
The invention is described in detail below by way of examples, which are intended to be within the scope of the claims. It should be noted that the following examples are only intended to illustrate the present invention and should not be construed as limiting the scope of the present invention, and that some insubstantial modifications and adaptations made in accordance with the present invention are still within the scope of the present invention.
Detailed Description
The present invention will be further described with reference to the following examples.
The raw materials or chemical reagents used in the examples of the present invention are commercially available unless otherwise specified.
Example 1
The main raw materials are as follows: hydrogen peroxide (hydrogen peroxide content 30.0%), polyvinyl alcohol 1799 type diluent (solid content 15.0%), antimony trioxide (content 99.5%), methyltrimethoxysilane (purity 99.0%), sodium bisulfate (15.0%), molybdenum trioxide sol (solid content 18.5%), sodium hydroxide (solid content 15.0%).
The preparation method comprises the following steps: adding 800L of water into a reaction kettle, adding 8.7 g of sodium bisulfate, dropwise adding 12.5 g of methyltrimethoxysilane under stirring at room temperature, stirring for 30 minutes, adding 35.1 g of polyvinyl alcohol solution, adding 180.2 g of antimony trioxide, heating to 75 ℃, dropwise adding 126.6 g of hydrogen peroxide, and continuing stirring for 1 hour after the solution is transparent; 32.5 g of sodium hydroxide solution is dropwise added, 120.9 g of self-made molybdenum trioxide solution is added, the measured solid content is 18.7%, the temperature is continuously raised to 95 ℃, the solution is distilled and concentrated to the required concentration, and the heating is stopped.
Example 2
The main raw materials are as follows: hydrogen peroxide (hydrogen peroxide content 30.0%), vinyl chloride-vinyl acetate copolymer emulsion (solid content 35.0%), antimony trioxide (content 99.5%), methyltrimethoxysilane and tetramethoxysilane (mass ratio 1: 1), molybdenum disulfide sol (solid content 26.0%) and sodium hydroxide solution (solid content 15.0%).
The preparation method comprises the following steps: adding 1500L of water into a reaction kettle, dropwise adding 32.5 g of a mixture of methyltrimethoxysilane and tetramethoxysilane under stirring at room temperature, stirring for 30 minutes, adding 25.3 g of polyvinyl chloride-vinyl acetate emulsion, adding 350.1 g of antimony trioxide, heating to 85 ℃, dropwise adding 245.8 g of hydrogen peroxide, and continuously stirring for 1.5 hours after the solution is transparent; and (3) dropwise adding 41.8 g of sodium hydroxide solution, adding 199.5 g of self-made molybdenum disulfide solution, actually measuring the solid content to be 20.4%, continuously heating to 95 ℃, concentrating the distilled excessive water to the required concentration, and stopping heating to finish the preparation.
Example 3
The main raw materials are as follows: hydrogen peroxide (hydrogen peroxide content 50.0%), potassium bisulfate (solid content 10.0%), aqueous brominated polyurethane and aqueous organic silicon modified acrylic acid mixed emulsion (self-made, solid content 35.0%), antimony trioxide (solid content 99.5%) and molybdenum disulfide sol (solid content 26.0%).
The preparation method comprises the following steps: adding 450.0 g of water into a reaction kettle, dropwise adding 14.5 g of potassium hydrogen sulfate while stirring at room temperature, stirring for 30 minutes, adding 45.3 g of aqueous brominated polyurethane and aqueous organic silicon modified acrylic acid mixed emulsion, adding 120.0 g of antimony trioxide, heating to 85 ℃, dropwise adding 72.0 g of hydrogen peroxide, and continuously stirring for 1 hour after the solution is transparent; adding 34.5 g of self-made molybdenum disulfide solution, actually measuring the solid content to be 21.5%, continuously heating to 100 ℃, concentrating the distilled excessive water to the required concentration, stopping heating, and finishing the preparation.

Claims (8)

1. The synthesis method of the antimony oxide sol and the flame retardant additive are characterized by comprising the following three steps of: uniformly dispersing water, a sol stabilizer, antimony trioxide, a modifier and the like, dropwise adding hydrogen peroxide, and heating the mixture to 70-95 ℃ to obtain an antimony oxide-containing mixture; adding a pH regulator, and adding one or two of molybdenum trioxide sol and molybdenum disulfide sol; and (3) concentrating to the required concentration.
2. The method for synthesizing antimony oxide sol and the flame retardant additive according to claim 1, wherein the method comprises the following steps: in the step (1), the sol stabilizer is one or a mixture of bisulfate and organic resin, and the modifier is a silane coupling agent; the molar ratio of the hydrogen peroxide to the antimony trioxide in the hydrogen peroxide is less than 2, and the preferred molar ratio is 1.60-1.99; the heating temperature is 70-95 ℃, and the reaction time is 2-6 hours.
3. The preparation method according to claim 2, wherein the modifier comprises one or more organic or inorganic agents containing silicon; which comprises tetramethoxysilane, phenyltrimethoxysilane, phenyltriethoxysilane, tetraethoxysilane, methyltrimethoxysilane, ethyltrimethoxysilane, ethyltriethoxysilane, propyltrimethoxysilane, dimethyldimethoxysilane, gamma-aminopropyltriethoxysilane, gamma-aminopropyltrimethoxysilane, gamma- (2, 3-glycidoxy) propyltrimethoxysilane, gamma-methacryloxypropyltrimethoxysilane, N- (beta-aminoethyl) -gamma-aminopropyltriethoxysilane, N-beta- (aminoethyl) -gamma-aminopropyltrimethoxysilane, N-beta- (aminoethyl) -gamma-aminopropylmethyldimethoxysilane, phenyltrimethoxysilane, phenyltriethoxysilane, tetraethoxysilane, methyltrimethoxysilane, ethyltrimethoxysilane, ethyltriethoxysilane, ethyltrimethoxysilane, propyltrimethoxysilane, dimethyldimethoxysilane, dimethyldimethoxy, One or more of gamma-aminopropylmethyldiethoxysilane, vinyltriethoxysilane, vinyltrimethoxysilane, vinyltris (beta-methoxyethoxy) silane, silica powder or silica sol; one or more of gamma-aminopropyltriethoxysilane, gamma-methacryloxypropyltrimethoxysilane, gamma- (2, 3-glycidoxy) propyltrimethoxysilane, silica powder or silica sol is preferably used.
4. The preparation method according to claim 2, wherein the sol stabilizer is one or more of hydrogen sulfate and organic resin, and the hydrogen sulfate is preferably sodium hydrogen sulfate; the organic resin can be dispersed in water, and comprises one or more of water-based halogen-free or halogen-containing saturated polyester, water-based halogen-free or halogen-containing unsaturated polyester, water-based halogen-free or halogen-containing polyurethane, water-based halogen-free or halogen-containing epoxy resin, water-based halogen-free or halogen-containing acrylic resin, water-based halogen-free or halogen-containing polyolefin resin, polyethylene glycol, polyvinylpyrrolidone, polyethylene oxide, polylactic acid and polyvinyl alcohol; the organic resin is capable of aqueous dispersion and has the following characteristics: the resin is soluble in water or a mixed solvent of water and alcohol; or the resin can be dissolved in an organic solvent, and the resulting solution can be dispersed in water with added surfactant to form a water-soluble emulsion.
5. The preparation method of claim 2, wherein the mass ratio of the water, the stabilizer, the antimony trioxide and the silane coupling agent is 3-8: 0.05-0.2: 1: 0.02 to 0.15; wherein the mass ratio of the sodium bisulfate to the solid content of the water-based resin is 1: 0.1 to 10.
6. The method for synthesizing a sol of antimony oxide and preparing a flame retardant aid according to claim 1, wherein the method comprises the following steps: adding one or two of molybdenum trioxide sol and molybdenum disulfide sol in the step (2), wherein the diameter of the nano particles in the sol is less than 200 nanometers, and the molybdenum trioxide sol is preferably selected; a PH adjusting agent comprising an alkali or alkaline earth metal hydroxide, preferably sodium hydroxide or potassium hydroxide.
7. The method for synthesizing a sol of antimony oxide and preparing a flame retardant aid according to claim 1, wherein the method comprises the following steps: firstly, dripping a PH regulator, and then adding one or two of molybdenum trioxide sol and molybdenum disulfide sol; the mass ratio of the total mass of the solids contained in the molybdenum trioxide or molybdenum disulfide sol to the total mass of the solids of the antimony oxide sol prepared in the step (1) is 0.05-0.2, and the preferred mass ratio is 0.1.
8. The method for synthesizing a sol of antimony oxide and preparing a flame retardant aid according to claim 1, wherein the method comprises the following steps: the concentration temperature of the liquid in the step (3) is 75-105 ℃; distillation under atmospheric or reduced pressure, preferably reduced pressure.
CN202010595627.1A 2020-06-28 2020-06-28 Synthesis method of antimony oxide sol and flame-retardant auxiliary Pending CN111748231A (en)

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Application publication date: 20201009