CN112028595A - Halogen-resistant inorganic flame-retardant floor and processing method thereof - Google Patents
Halogen-resistant inorganic flame-retardant floor and processing method thereof Download PDFInfo
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- CN112028595A CN112028595A CN202010837710.5A CN202010837710A CN112028595A CN 112028595 A CN112028595 A CN 112028595A CN 202010837710 A CN202010837710 A CN 202010837710A CN 112028595 A CN112028595 A CN 112028595A
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B28/00—Compositions of mortars, concrete or artificial stone, containing inorganic binders or the reaction product of an inorganic and an organic binder, e.g. polycarboxylate cements
- C04B28/30—Compositions of mortars, concrete or artificial stone, containing inorganic binders or the reaction product of an inorganic and an organic binder, e.g. polycarboxylate cements containing magnesium cements or similar cements
- C04B28/32—Magnesium oxychloride cements, e.g. Sorel cement
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B28—WORKING CEMENT, CLAY, OR STONE
- B28B—SHAPING CLAY OR OTHER CERAMIC COMPOSITIONS; SHAPING SLAG; SHAPING MIXTURES CONTAINING CEMENTITIOUS MATERIAL, e.g. PLASTER
- B28B11/00—Apparatus or processes for treating or working the shaped or preshaped articles
- B28B11/24—Apparatus or processes for treating or working the shaped or preshaped articles for curing, setting or hardening
- B28B11/245—Curing concrete articles
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B28—WORKING CEMENT, CLAY, OR STONE
- B28B—SHAPING CLAY OR OTHER CERAMIC COMPOSITIONS; SHAPING SLAG; SHAPING MIXTURES CONTAINING CEMENTITIOUS MATERIAL, e.g. PLASTER
- B28B23/00—Arrangements specially adapted for the production of shaped articles with elements wholly or partly embedded in the moulding material; Production of reinforced objects
- B28B23/02—Arrangements specially adapted for the production of shaped articles with elements wholly or partly embedded in the moulding material; Production of reinforced objects wherein the elements are reinforcing members
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B14/00—Use of inorganic materials as fillers, e.g. pigments, for mortars, concrete or artificial stone; Treatment of inorganic materials specially adapted to enhance their filling properties in mortars, concrete or artificial stone
- C04B14/02—Granular materials, e.g. microballoons
- C04B14/022—Carbon
- C04B14/026—Carbon of particular shape, e.g. nanotubes
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B14/00—Use of inorganic materials as fillers, e.g. pigments, for mortars, concrete or artificial stone; Treatment of inorganic materials specially adapted to enhance their filling properties in mortars, concrete or artificial stone
- C04B14/02—Granular materials, e.g. microballoons
- C04B14/04—Silica-rich materials; Silicates
- C04B14/20—Mica; Vermiculite
- C04B14/202—Vermiculite
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B40/00—Processes, in general, for influencing or modifying the properties of mortars, concrete or artificial stone compositions, e.g. their setting or hardening ability
- C04B40/0028—Aspects relating to the mixing step of the mortar preparation
- C04B40/0039—Premixtures of ingredients
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2111/00—Mortars, concrete or artificial stone or mixtures to prepare them, characterised by specific function, property or use
- C04B2111/20—Resistance against chemical, physical or biological attack
- C04B2111/27—Water resistance, i.e. waterproof or water-repellent materials
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2111/00—Mortars, concrete or artificial stone or mixtures to prepare them, characterised by specific function, property or use
- C04B2111/20—Resistance against chemical, physical or biological attack
- C04B2111/28—Fire resistance, i.e. materials resistant to accidental fires or high temperatures
Abstract
The invention discloses a halogen-resistant inorganic flame-retardant floor and a processing method thereof, wherein the halogen-resistant inorganic flame-retardant floor comprises the following raw materials in parts by weight: 20-30 parts of magnesium chloride, 20-30 parts of magnesium oxide, 5-10 parts of flame-retardant filler and 3-8 parts of waterproof additive; the flame-retardant filler is prepared by embedding pre-modified vermiculite loaded with nano aluminum hydroxide and nano magnesium hydroxide on an activated multi-walled carbon nanotube, and a glass magnesium board is used as a base material, so that the glass magnesium board has a good flame-retardant effect, and various inorganic flame retardants are used in a matching manner, so that the prepared inorganic flame-retardant floor has good flame retardance, and a waterproof additive is prepared, and is reacted with hydroxyl on the surface of the glass magnesium board to dehydrate molecules to form a Si-O-Si main chain, so that a layer of hydrophobic film is formed on the surface of a bottom plate, and further the anti-halogenation effect is achieved.
Description
Technical Field
The invention belongs to the technical field of floor processing, and particularly relates to a halogen-resistant inorganic flame-retardant floor and a processing method thereof.
Background
Floor, i.e. the surface layer of the floor or floor of a house. Made of wood or other material. There are many classifications of floors, classified by structure: solid wood floors, laminate wood floors, three-layer solid wood laminate floors, bamboo and wood floors, anti-corrosion floors, cork floors, and the most popular multilayer solid wood laminate floors; classified by use are: household, commercial usefulness, antistatic floor, outdoor floor, the special floor of stage dance, special floor in sports hall, the special floor in track and field etc. along with the wide use of bottom plate, people also improve increasingly to its fire-retardant fire-resistant demand.
The flame retardant effect of the existing flame retardant floor is general, and the floor can not be instantly burnt when meeting naked flame or under the action of high temperature in the air, but can be burnt when being acted by naked flame or high temperature for a long time, and the floor can have the phenomenon of anti-halogen in the use process due to poor self waterproof property, so that the flame retardant floor can not be normally used.
Disclosure of Invention
The invention aims to provide a halogen-resistant inorganic flame-retardant floor and a processing method thereof.
The technical problems to be solved by the invention are as follows:
the flame retardant effect of the existing flame retardant floor is general, and the floor can not be instantly burnt when meeting naked flame or under the action of high temperature in the air, but can be burnt when being acted by naked flame or high temperature for a long time, and the floor can have the phenomenon of anti-halogen in the use process due to poor self waterproof property, so that the flame retardant floor can not be normally used.
The purpose of the invention can be realized by the following technical scheme:
the halogen-resistant inorganic flame-retardant floor comprises the following raw materials in parts by weight: 20-30 parts of magnesium chloride, 20-30 parts of magnesium oxide, 5-10 parts of flame-retardant filler and 3-8 parts of waterproof additive;
the halogenated-resistant inorganic flame-retardant floor is prepared by the following steps:
step S1: adding magnesium chloride and deionized water into a reaction kettle, stirring until the magnesium chloride is completely dissolved to prepare a magnesium chloride solution with the Baume degree of 20-26, and standing for 20-25 h;
step S2: adding magnesium oxide, flame-retardant filler, waterproof additive and magnesium chloride solution into a stirring kettle, and stirring until the mixture is uniformly mixed under the condition that the rotating speed is 300-500r/min to prepare slurry;
step S3: laying a layer of non-woven fabric and a layer of alkali-free glass fiber fabric at the bottom of the mold, pouring the slurry prepared in the step S2 for molding, laying a layer of alkali-free glass fiber fabric and a layer of non-woven fabric, and drying at the temperature of 25-30 ℃ for 3-5 days to prepare a glass magnesium substrate;
step S4: and (4) moving the glass magnesium substrate prepared in the step (S3) into a curing chamber, curing for 20-30 days at the temperature of 45-55 ℃ and the humidity of 20-30%, moving the glass magnesium substrate out every 15-20h during curing, fumigating for 30-40min by using nitrogen loaded with 4-6% of trimethylaluminum by volume fraction, then placing into the curing chamber, and continuing to cure until the end to obtain the halogenated-resistant inorganic flame-retardant floor.
Further, the flame-retardant filler is prepared by the following steps:
step A1: adding the multi-walled carbon nano-tube into mixed acid, soaking for 30-40min, filtering to remove the mixed acid, adding a filter cake into dimethyl sulfoxide, stirring at the rotation speed of 300-500r/min until the filter cake is uniformly dispersed, adding dicyclohexylcarbodiimide, continuously stirring for 3-4h, and filtering again to remove the filtrate to obtain the activated multi-walled carbon nano-tube;
step A2: adding vermiculite and sodium chloride solution into a reaction kettle, stirring for 2-3h at the conditions of the rotation speed of 300-40 ℃ and the temperature of 35-40 ℃, filtering to remove filtrate, washing a filter cake with deionized water until no chloride ions remain on the surface, adding the filter cake and tetramethylammonium bromide solution into the stirring kettle, stirring for 30-40min at the rotation speed of 100-150r/min and the temperature of 50-60 ℃, removing the tetramethylammonium bromide solution, adding a hexadecyltrimethylammonium bromide solution, continuously stirring for 2-3h at the temperature of 80-85 ℃, filtering to remove the filtrate, and drying the filter cake at the temperature of 110-120 ℃ to prepare a vermiculite matrix;
step A3: adding boric acid and dimethylformamide into a reaction kettle, stirring until the boric acid is completely dissolved, adding phosphoric acid, continuously stirring until the boric acid is uniformly mixed to prepare an addition solution, adding the addition solution and urea into the reaction kettle, stirring for 3-5min under the conditions that the rotating speed is 100-;
step A4: adding nanometer aluminum hydroxide, nanometer magnesium hydroxide and deionized water into a reaction kettle, stirring until the nanometer aluminum hydroxide and the nanometer magnesium hydroxide are completely dispersed, adding liquid paraffin and fatty glyceride, continuously stirring for 30-40min at the rotation speed of 5000-, adding the pre-modified vermiculite prepared in the step A3, continuously stirring for 20-30min, filtering to remove filtrate, drying a filter cake at the temperature of 120-130 ℃, adding the filter cake into deionized water until the filter cake is uniformly dispersed, adding the activated multi-walled carbon nano-tube prepared in the step A1, ultrasonic treatment is carried out for 30-50min under the condition of the frequency of 2-5MHz, filtering to remove the filtrate, and preserving the temperature of the filter cake for 2-3h at the temperature of 200-230 ℃ to obtain the flame-retardant filler.
Further, the mixed acid in the step A1 is prepared by mixing concentrated sulfuric acid and concentrated nitric acid in a volume ratio of 3:1, the mass fraction of the concentrated sulfuric acid is 75-80%, the mass fraction of the concentrated nitric acid is 70-75%, the dosage ratio of the filter cake to dimethyl sulfoxide is 5g:1mL, the dosage of dicyclohexylcarbodiimide is 45-50% of the mass of the filter cake, the concentration of the sodium chloride solution in the step A2 is 3-5mol/L, the concentration of the tetramethylammonium bromide solution is 1-1.5mol/L, the concentration of the hexadecyltrimethylammonium bromide solution is 2-5mol/L, the dosage of boric acid, phosphoric acid and urea in the step A3 is 1:1:1.8-2, the dosage of nano aluminum hydroxide and nano magnesium hydroxide in the step A4 is 1:1, and the dosage of liquid paraffin is 2-4% of the sum of the mass of the nano aluminum hydroxide and the nano magnesium hydroxide, the dosage of the fatty glyceride is 3-4% of the mass sum of the nano aluminum hydroxide and the nano magnesium hydroxide, the dosage of the pre-modified vermiculite is 5-8 times of the mass sum of the nano aluminum hydroxide and the nano magnesium hydroxide, and the dosage mass ratio of the filter cake to the activated multi-wall carbon nano tube is 2-2.5: 8.
Further, the waterproof additive is prepared by the following steps:
step B1: adding n-butyl titanate into isopropanol to mix until the n-butyl titanate is uniformly mixed, adding deionized water, stirring for 30-40min under the condition that the rotation speed is 120r/min, distilling for 10-15min under the condition that the temperature is 85-90 ℃, drying a substrate under the condition that the temperature is 60-80 ℃, and roasting for 2-3h under the condition that the temperature is 600 ℃ to prepare the nano titanium dioxide;
step B2: adding deionized water and sodium dodecyl benzene sulfonate into a reaction kettle, stirring at the rotation speed of 300-500r/min and the temperature of 50-60 ℃ until the sodium dodecyl benzene sulfonate is completely dissolved, adding fatty alcohol-polyoxyethylene ether and the nano titanium dioxide prepared in the step B1, stirring at the temperature of 70-80 ℃ for 10-15min, adding octamethylcyclotetrasiloxane, adjusting the pH value to 2-3, and stirring for 3-5h to prepare a mixed emulsion;
step B3: adding deionized water and silicon powder into a reaction kettle, stirring for 5-10min at the rotation speed of 800-1000r/min, adding sodium hydroxide, stirring for 6-8h at the temperature of 85-90 ℃, cooling to 40-45 ℃, standing for 10-15h to obtain silica sol, adding the silica sol and the mixed emulsion into the stirring kettle, and performing ultrasonic treatment for 2-3h at the frequency of 30-50kHz and the temperature of 35-40 ℃ to obtain the waterproof additive.
Further, the volume ratio of the n-butyl titanate, the isopropanol and the deionized water in the step B1 is 13-15:20:3-5, the mass ratio of the deionized water, the sodium dodecyl benzene sulfonate, the fatty alcohol polyoxyethylene ether, the nano titanium dioxide and the octamethylcyclotetrasiloxane in the step B2 is 10:2:2-2.5:1-1.3:1.5-2, and the mass ratio of the deionized water, the silicon powder and the sodium hydroxide in the step B3 is 200:25: 0.15-0.2.
A processing method of a halogen-resistant inorganic flame-retardant floor specifically comprises the following steps:
step S1: adding magnesium chloride and deionized water into a reaction kettle, stirring until the magnesium chloride is completely dissolved to prepare a magnesium chloride solution with the Baume degree of 20-26, and standing for 20-25 h;
step S2: adding magnesium oxide, flame-retardant filler, waterproof additive and magnesium chloride solution into a stirring kettle, and stirring until the mixture is uniformly mixed under the condition that the rotating speed is 300-500r/min to prepare slurry;
step S3: laying a layer of non-woven fabric and a layer of alkali-free glass fiber fabric at the bottom of the mold, pouring the slurry prepared in the step S2 for molding, laying a layer of alkali-free glass fiber fabric and a layer of non-woven fabric, and drying at the temperature of 25-30 ℃ for 3-5 days to prepare a glass magnesium substrate;
step S4: and (4) moving the glass magnesium substrate prepared in the step (S3) into a curing chamber, curing for 20-30 days at the temperature of 45-55 ℃ and the humidity of 20-30%, moving the glass magnesium substrate out every 15-20h during curing, fumigating for 30-40min by using nitrogen loaded with 4-6% of trimethylaluminum by volume fraction, then placing into the curing chamber, and continuing to cure until the end to obtain the halogenated-resistant inorganic flame-retardant floor.
The invention has the beneficial effects that: the invention prepares a flame-retardant filler in the process of preparing an anti-halogenation inorganic flame-retardant floor, the flame-retardant filler takes multi-walled carbon nano-tubes as raw materials, the multi-walled carbon nano-tubes have good flame-retardant effect and can form a continuous protective carbon layer with a grid structure during combustion so as to prevent combustion, the multi-walled carbon nano-tubes are treated by mixed acid so as to increase surface etching, a large amount of carboxyl is introduced on the surface, dicyclohexyl carbodiimide is further used for treatment so as to activate the carboxyl on the surface, vermiculite is treated by sodium chloride solution so as to exchange surface ions and sodium ions of vermiculite, the vermiculite is expanded by tetramethyl ammonium bromide solution and hexadecyl trimethyl ammonium bromide solution in sequence so as to organize the vermiculite, boric acid is dissolved in dimethyl formamide and added with phosphoric acid for mixing to prepare an additive solution, and then urea and the vermiculite are added so as to enable the boric acid solution and the phosphoric acid solution to respectively react with the vermiculite, leading a large amount of active groups to be introduced into the surface of the vermiculite, further carrying out polycondensation reaction with urea, wherein the vermiculite belongs to 2:1 type layered silicate, each unit cell is formed by clamping a layer of brucite octahedron between two layers of silicon-oxygen tetrahedrons, the brucite octahedron is connected between the two layers of silicon-oxygen tetrahedrons by sharing oxygen atoms, active hydroxyl groups between the layers are exposed after organic treatment, a large amount of pores are formed, the active hydroxyl groups are partially reacted with boric acid and phosphoric acid, the residual hydroxyl groups are still exposed on the surface, nano aluminum hydroxide and nano magnesium hydroxide are subjected to surface treatment by using fatty glyceride, so that the dispersibility of the nano aluminum hydroxide and the nano magnesium hydroxide is improved, the surface of the nano aluminum hydroxide and the nano magnesium hydroxide has activity, further the nano aluminum hydroxide and the nano magnesium hydroxide are mixed with pre-modified vermiculite, the activated multi-walled carbon nanotube and a filter cake are subjected to ultrasonic treatment, so that, and then embedding the pre-modified vermiculite loaded with nano aluminum hydroxide and nano magnesium hydroxide on an activated multi-walled carbon nanotube to prepare a flame retardant filler, and taking a glass magnesium board as a base material, wherein the glass magnesium board has a good flame retardant effect, and multiple inorganic flame retardants are matched for use, so that the prepared inorganic flame retardant floor has good flame retardancy, and a waterproof additive is prepared, wherein the waterproof additive is a mixed emulsion prepared from nano titanium dioxide and octamethylcyclotetrasiloxane, the mixed emulsion is an organic silicon emulsion and contains a large amount of nano silicon dioxide, the mixed emulsion is further dissolved and mixed with silica gel to obtain a waterproof additive, the waterproof additive reacts with hydroxyl on the surface of the glass magnesium board to dehydrate molecules to form a Si-O-Si main chain, and a layer of hydrophobic film is formed on the surface of the bottom board, so that the anti-halogenation effect is achieved.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1
The halogen-resistant inorganic flame-retardant floor comprises the following raw materials in parts by weight: 20 parts of magnesium chloride, 20 parts of magnesium oxide, 5 parts of flame-retardant filler and 3 parts of waterproof additive;
the halogenated-resistant inorganic flame-retardant floor is prepared by the following steps:
step S1: adding magnesium chloride and deionized water into a reaction kettle, stirring until the magnesium chloride is completely dissolved to prepare a magnesium chloride solution with the Baume degree of 20, and standing for 20 hours;
step S2: adding magnesium oxide, flame-retardant filler, waterproof additive and magnesium chloride solution into a stirring kettle, and stirring until the mixture is uniformly mixed under the condition that the rotating speed is 300r/min to prepare slurry;
step S3: laying a layer of non-woven fabric and a layer of alkali-free glass fiber fabric at the bottom of the mold, pouring the slurry prepared in the step S2 for molding, laying a layer of alkali-free glass fiber fabric and a layer of non-woven fabric, and drying at the temperature of 25 ℃ for 3 days to prepare a glass magnesium substrate;
step S4: and (4) moving the glass magnesium substrate prepared in the step (S3) into a curing chamber, curing for 20 days at the temperature of 45 ℃ and the humidity of 20%, moving the glass magnesium substrate out every 15h during curing, fumigating for 30min by using nitrogen loaded with trimethylaluminum with the volume fraction of 4%, then placing the glass magnesium substrate into the curing chamber, and continuing curing until the end to obtain the halogenated-resistant inorganic flame-retardant floor.
The flame-retardant filler is prepared by the following steps:
step A1: adding the multi-walled carbon nanotube into mixed acid, soaking for 30min, filtering to remove the mixed acid, adding a filter cake into dimethyl sulfoxide, stirring at the rotation speed of 300r/min until the filter cake is uniformly dispersed, adding dicyclohexylcarbodiimide, continuously stirring for 3h, and filtering again to remove filtrate to obtain an activated multi-walled carbon nanotube;
step A2: adding vermiculite and sodium chloride solution into a reaction kettle, stirring for 2 hours at the conditions of the rotating speed of 300r/min and the temperature of 35 ℃, filtering to remove filtrate, washing a filter cake with deionized water until no chloride ions remain on the surface, adding the filter cake and tetramethylammonium bromide solution into the reaction kettle, stirring for 30 minutes at the rotating speed of 100r/min and the temperature of 50 ℃, removing the tetramethylammonium bromide solution, adding a hexadecyltrimethylammonium bromide solution, continuously stirring for 2 hours at the temperature of 80 ℃, filtering to remove the filtrate, and drying the filter cake at the temperature of 110 ℃ to obtain a vermiculite matrix;
step A3: adding boric acid and dimethylformamide into a reaction kettle, stirring until the boric acid is completely dissolved, adding phosphoric acid, continuously stirring until the boric acid is uniformly mixed to prepare an addition solution, adding the addition solution and urea into the reaction kettle, stirring for 3min at the rotation speed of 100r/min and the temperature of 25 ℃, heating to 130 ℃ at the speed of 5 ℃/min, stirring for 10min, adding the vermiculite matrix prepared in the step A2, continuously stirring for 30min, filtering to remove filtrate, and heating a filter cake for 2h at the temperature of 220 ℃ to prepare pre-modified vermiculite;
step A4: adding nano aluminum hydroxide, nano magnesium hydroxide and deionized water into a reaction kettle, stirring until the nano aluminum hydroxide and the nano magnesium hydroxide are completely dispersed, adding liquid paraffin and fatty glyceride, continuously stirring for 30min at the rotation speed of 5000r/min and the temperature of 80 ℃, adding the pre-modified vermiculite prepared in the step A3, continuously stirring for 20min, filtering to remove filtrate, drying the filter cake at the temperature of 120 ℃, adding the filter cake into the deionized water until the filter cake is uniformly dispersed, adding the activated multi-walled carbon nano tube prepared in the step A1, carrying out ultrasonic treatment for 30min at the frequency of 2MHz, filtering to remove the filtrate, and carrying out heat preservation for 2h at the temperature of 200 ℃ to prepare the flame retardant filler.
The waterproof additive is prepared by the following steps:
step B1: adding n-butyl titanate into isopropanol, mixing until the n-butyl titanate and the isopropanol are uniformly mixed, adding deionized water, stirring for 30min at the rotation speed of 100r/min, distilling for 10min at the temperature of 85 ℃, drying a substrate at the temperature of 60 ℃, and roasting for 2h at the temperature of 500 ℃ to obtain the nano titanium dioxide;
step B2: adding deionized water and sodium dodecyl benzene sulfonate into a reaction kettle, stirring at the rotation speed of 300r/min and the temperature of 50 ℃ until the sodium dodecyl benzene sulfonate is completely dissolved, adding fatty alcohol-polyoxyethylene ether and the nano titanium dioxide prepared in the step B1, stirring at the temperature of 70 ℃ for 10min, adding octamethylcyclotetrasiloxane, adjusting the pH value to be 2, and stirring for 3h to prepare a mixed emulsion;
step B3: adding deionized water and silicon powder into a reaction kettle, stirring for 5min at the rotation speed of 800r/min, adding sodium hydroxide, stirring for 6h at the temperature of 85 ℃, cooling to 40 ℃, standing for 10h to prepare silica sol, adding the silica sol and the mixed emulsion into the stirring kettle, and carrying out ultrasonic treatment for 2h at the frequency of 30kHz and the temperature of 35 ℃ to prepare the waterproof additive.
Example 2
The halogen-resistant inorganic flame-retardant floor comprises the following raw materials in parts by weight: 25 parts of magnesium chloride, 25 parts of magnesium oxide, 8 parts of flame-retardant filler and 5 parts of waterproof additive;
the halogenated-resistant inorganic flame-retardant floor is prepared by the following steps:
step S1: adding magnesium chloride and deionized water into a reaction kettle, stirring until the magnesium chloride is completely dissolved to prepare a magnesium chloride solution with a Baume degree of 24, and standing for 23 hours;
step S2: adding magnesium oxide, flame-retardant filler, waterproof additive and magnesium chloride solution into a stirring kettle, and stirring until the mixture is uniformly mixed under the condition that the rotating speed is 400r/min to prepare slurry;
step S3: laying a layer of non-woven fabric and a layer of alkali-free glass fiber fabric at the bottom of the mold, pouring the slurry prepared in the step S2 for molding, laying a layer of alkali-free glass fiber fabric and a layer of non-woven fabric, and drying at the temperature of 28 ℃ for 4 days to prepare a glass magnesium substrate;
step S4: and (4) moving the glass magnesium substrate prepared in the step (S3) into a curing chamber, curing for 25 days at the temperature of 50 ℃ and the humidity of 25%, moving the glass magnesium substrate out every 18 hours during curing, fumigating for 35min by using nitrogen loaded with trimethylaluminum with the volume fraction of 5%, then placing the glass magnesium substrate into the curing chamber, and continuing curing until the end to obtain the halogenated-resistant inorganic flame-retardant floor.
The flame-retardant filler is prepared by the following steps:
step A1: adding the multi-walled carbon nanotube into mixed acid, soaking for 35min, filtering to remove the mixed acid, adding a filter cake into dimethyl sulfoxide, stirring at the rotation speed of 400r/min until the filter cake is uniformly dispersed, adding dicyclohexylcarbodiimide, continuously stirring for 4h, and filtering again to remove filtrate to obtain an activated multi-walled carbon nanotube;
step A2: adding vermiculite and sodium chloride solution into a reaction kettle, stirring for 2.5 hours at the rotation speed of 400r/min and the temperature of 38 ℃, filtering to remove filtrate, washing a filter cake with deionized water until no chloride ions remain on the surface, adding the filter cake and tetramethylammonium bromide solution into the reaction kettle, stirring for 35 minutes at the rotation speed of 120r/min and the temperature of 55 ℃, removing the tetramethylammonium bromide solution, adding a hexadecyltrimethylammonium bromide solution, stirring for 2.5 hours at the temperature of 93 ℃, filtering to remove the filtrate, and drying the filter cake at the temperature of 115 ℃ to obtain a vermiculite matrix;
step A3: adding boric acid and dimethylformamide into a reaction kettle, stirring until the boric acid is completely dissolved, adding phosphoric acid, continuously stirring until the boric acid is uniformly mixed to prepare an addition solution, adding the addition solution and urea into the reaction kettle, stirring for 4min at the rotation speed of 130r/min and the temperature of 28 ℃, heating to the temperature of 135 ℃ at the speed of 6 ℃/min, stirring for 13min, adding the vermiculite matrix prepared in the step A2, continuously stirring for 40min, filtering to remove filtrate, and heating a filter cake for 2h at the temperature of 240 ℃ to prepare pre-modified vermiculite;
step A4: adding nano aluminum hydroxide, nano magnesium hydroxide and deionized water into a reaction kettle, stirring until the nano aluminum hydroxide and the nano magnesium hydroxide are completely dispersed, adding liquid paraffin and fatty glyceride, continuously stirring for 35min at the rotation speed of 5000r/min and the temperature of 85 ℃, adding the pre-modified vermiculite prepared in the step A3, continuously stirring for 25min, filtering to remove filtrate, drying the filter cake at the temperature of 125 ℃, adding the filter cake into the deionized water until the filter cake is uniformly dispersed, adding the activated multi-walled carbon nanotube prepared in the step A1, carrying out ultrasonic treatment for 40min at the frequency of 4MHz, filtering to remove the filtrate, and carrying out heat preservation for 2h at the temperature of 220 ℃ to prepare the flame retardant filler.
The waterproof additive is prepared by the following steps:
step B1: adding n-butyl titanate into isopropanol, mixing until the n-butyl titanate and the isopropanol are uniformly mixed, adding deionized water, stirring for 35min at the rotation speed of 110r/min, distilling for 13min at the temperature of 88 ℃, drying a substrate at the temperature of 70 ℃, and roasting for 2h at the temperature of 550 ℃ to obtain the nano titanium dioxide;
step B2: adding deionized water and sodium dodecyl benzene sulfonate into a reaction kettle, stirring until the sodium dodecyl benzene sulfonate is completely dissolved at the rotation speed of 400r/min and the temperature of 55 ℃, adding fatty alcohol-polyoxyethylene ether and the nano titanium dioxide prepared in the step B1, stirring for 13min at the temperature of 75 ℃, adding octamethylcyclotetrasiloxane, adjusting the pH value to be 2, and stirring for 4h to prepare a mixed emulsion;
step B3: adding deionized water and silicon powder into a reaction kettle, stirring for 8min at the rotation speed of 900r/min, adding sodium hydroxide, stirring for 7h at the temperature of 88 ℃, cooling to 43 ℃, standing for 13h to obtain silica sol, adding the silica sol and the mixed emulsion into the stirring kettle, and performing ultrasonic treatment for 2h at the frequency of 40kHz and the temperature of 38 ℃ to obtain the waterproof additive.
Example 3
The halogen-resistant inorganic flame-retardant floor comprises the following raw materials in parts by weight: 30 parts of magnesium chloride, 30 parts of magnesium oxide, 10 parts of flame-retardant filler and 8 parts of waterproof additive;
the halogenated-resistant inorganic flame-retardant floor is prepared by the following steps:
step S1: adding magnesium chloride and deionized water into a reaction kettle, stirring until the magnesium chloride is completely dissolved to prepare a magnesium chloride solution with the Baume degree of 26, and standing for 25 hours;
step S2: adding magnesium oxide, flame-retardant filler, waterproof additive and magnesium chloride solution into a stirring kettle, and stirring at the rotation speed of 500r/min until the mixture is uniformly mixed to prepare slurry;
step S3: laying a layer of non-woven fabric and a layer of alkali-free glass fiber fabric at the bottom of the mold, pouring the slurry prepared in the step S2 for molding, laying a layer of alkali-free glass fiber fabric and a layer of non-woven fabric, and drying at the temperature of 30 ℃ for 5 days to prepare a glass magnesium substrate;
step S4: and (4) moving the glass magnesium substrate prepared in the step (S3) into a curing chamber, curing for 30 days at the temperature of 55 ℃ and the humidity of 30%, moving the glass magnesium substrate out every 20h during curing, fumigating for 40min by using nitrogen loaded with 6% by volume of trimethylaluminum, then placing the glass magnesium substrate into the curing chamber, and continuing curing until the end to obtain the halogenated-resistant inorganic flame-retardant floor.
The flame-retardant filler is prepared by the following steps:
step A1: adding the multi-walled carbon nanotube into mixed acid, soaking for 40min, filtering to remove the mixed acid, adding a filter cake into dimethyl sulfoxide, stirring at the rotation speed of 500r/min until the filter cake is uniformly dispersed, adding dicyclohexylcarbodiimide, continuously stirring for 4h, and filtering again to remove filtrate to obtain an activated multi-walled carbon nanotube;
step A2: adding vermiculite and sodium chloride solution into a reaction kettle, stirring for 3 hours at the conditions of the rotating speed of 500r/min and the temperature of 40 ℃, filtering to remove filtrate, washing a filter cake with deionized water until no chloride ions remain on the surface, adding the filter cake and tetramethylammonium bromide solution into the reaction kettle, stirring for 40 minutes at the rotating speed of 150r/min and the temperature of 60 ℃, removing the tetramethylammonium bromide solution, adding a hexadecyltrimethylammonium bromide solution, continuously stirring for 3 hours at the temperature of 85 ℃, filtering to remove the filtrate, and drying the filter cake at the temperature of 120 ℃ to obtain a vermiculite matrix;
step A3: adding boric acid and dimethylformamide into a reaction kettle, stirring until the boric acid is completely dissolved, adding phosphoric acid, continuously stirring until the boric acid is uniformly mixed to prepare an addition solution, adding the addition solution and urea into the reaction kettle, stirring for 5min at the rotation speed of 150r/min and the temperature of 30 ℃, heating to the temperature of 140 ℃ at the speed of 8 ℃/min, stirring for 15min, adding the vermiculite matrix prepared in the step A2, continuously stirring for 50min, filtering to remove filtrate, and heating a filter cake for 2-3h at the temperature of 250 ℃ to prepare pre-modified vermiculite;
step A4: adding nano aluminum hydroxide, nano magnesium hydroxide and deionized water into a reaction kettle, stirring until the nano aluminum hydroxide and the nano magnesium hydroxide are completely dispersed, adding liquid paraffin and fatty glyceride, continuously stirring for 40min at the rotation speed of 6000r/min and the temperature of 90 ℃, adding the pre-modified vermiculite prepared in the step A3, continuously stirring for 30min, filtering to remove filtrate, drying the filter cake at the temperature of 130 ℃, adding the filter cake into the deionized water until the filter cake is uniformly dispersed, adding the activated multi-walled carbon nano tube prepared in the step A1, carrying out ultrasonic treatment for 50min at the frequency of 5MHz, filtering to remove the filtrate, and carrying out heat preservation for 3h to prepare the flame retardant filler.
The waterproof additive is prepared by the following steps:
step B1: adding n-butyl titanate into isopropanol, mixing until the n-butyl titanate and the isopropanol are uniformly mixed, adding deionized water, stirring for 40min at the rotation speed of 120r/min, distilling for 15min at the temperature of 90 ℃, drying a substrate at the temperature of 80 ℃, and roasting for 3h at the temperature of 600 ℃ to obtain the nano titanium dioxide;
step B2: adding deionized water and sodium dodecyl benzene sulfonate into a reaction kettle, stirring at the rotation speed of 500r/min and the temperature of 60 ℃ until the sodium dodecyl benzene sulfonate is completely dissolved, adding fatty alcohol-polyoxyethylene ether and the nano titanium dioxide prepared in the step B1, stirring at the temperature of 80 ℃ for 15min, adding octamethylcyclotetrasiloxane, adjusting the pH value to 3, and stirring for 3-5h to prepare a mixed emulsion;
step B3: adding deionized water and silicon powder into a reaction kettle, stirring for 10min at the rotation speed of 1000r/min, adding sodium hydroxide, stirring for 8h at the temperature of 90 ℃, cooling to 45 ℃, standing for 15h to prepare silica sol, adding the silica sol and the mixed emulsion into the stirring kettle, and carrying out ultrasonic treatment for 3h at the frequency of 50kHz and the temperature of 40 ℃ to prepare the waterproof additive.
Comparative example
The comparative example is a common flame-retardant floor in the market.
The performance tests were performed on the flame retardant flooring obtained in examples 1 to 3 and comparative example, and the test results are shown in table 1 below;
TABLE 1
As can be seen from Table 1 above, the flame retardant grades of the flame retardant floorings prepared in examples 1-3 are all A1, while the flame retardant grade of the flame retardant flooring prepared in comparative example is B1, the flame retardant floorings prepared in examples 1-3 still do not absorb a lot of water after being soaked for 90min, and the flame retardant flooring prepared in comparative example absorbs a lot of water after being soaked for 60min, which shows that the flame retardant flooring has good flame retardancy and water resistance.
The foregoing is merely exemplary and illustrative of the principles of the present invention and various modifications, additions and substitutions of the specific embodiments described herein may be made by those skilled in the art without departing from the principles of the present invention or exceeding the scope of the claims set forth herein.
Claims (6)
1. The halogen-resistant inorganic flame-retardant floor is characterized in that: the feed comprises the following raw materials in parts by weight: 20-30 parts of magnesium chloride, 20-30 parts of magnesium oxide, 5-10 parts of flame-retardant filler and 3-8 parts of waterproof additive;
the halogenated-resistant inorganic flame-retardant floor is prepared by the following steps:
step S1: adding magnesium chloride and deionized water into a reaction kettle, stirring until the magnesium chloride is completely dissolved to prepare a magnesium chloride solution with the Baume degree of 20-26, and standing for 20-25 h;
step S2: adding magnesium oxide, flame-retardant filler, waterproof additive and magnesium chloride solution into a stirring kettle, and stirring until the mixture is uniformly mixed under the condition that the rotating speed is 300-500r/min to prepare slurry;
step S3: laying a layer of non-woven fabric and a layer of alkali-free glass fiber fabric at the bottom of the mold, pouring the slurry prepared in the step S2 for molding, laying a layer of alkali-free glass fiber fabric and a layer of non-woven fabric, and drying at the temperature of 25-30 ℃ for 3-5 days to prepare a glass magnesium substrate;
step S4: and (4) moving the glass magnesium substrate prepared in the step (S3) into a curing chamber, curing for 20-30 days at the temperature of 45-55 ℃ and the humidity of 20-30%, moving the glass magnesium substrate out every 15-20h during curing, fumigating for 30-40min by using nitrogen loaded with 4-6% of trimethylaluminum by volume fraction, then placing into the curing chamber, and continuing to cure until the end to obtain the halogenated-resistant inorganic flame-retardant floor.
2. The anti-halogenation inorganic fire-retardant floor according to claim 1, wherein: the flame-retardant filler is prepared by the following steps:
step A1: adding the multi-walled carbon nano-tube into mixed acid, soaking for 30-40min, filtering to remove the mixed acid, adding a filter cake into dimethyl sulfoxide, stirring at the rotation speed of 300-500r/min until the filter cake is uniformly dispersed, adding dicyclohexylcarbodiimide, continuously stirring for 3-4h, and filtering again to remove the filtrate to obtain the activated multi-walled carbon nano-tube;
step A2: adding vermiculite and sodium chloride solution into a reaction kettle, stirring for 2-3h at the conditions of the rotation speed of 300-40 ℃ and the temperature of 35-40 ℃, filtering to remove filtrate, washing a filter cake with deionized water until no chloride ions remain on the surface, adding the filter cake and tetramethylammonium bromide solution into the stirring kettle, stirring for 30-40min at the rotation speed of 100-150r/min and the temperature of 50-60 ℃, removing the tetramethylammonium bromide solution, adding a hexadecyltrimethylammonium bromide solution, continuously stirring for 2-3h at the temperature of 80-85 ℃, filtering to remove the filtrate, and drying the filter cake at the temperature of 110-120 ℃ to prepare a vermiculite matrix;
step A3: adding boric acid and dimethylformamide into a reaction kettle, stirring until the boric acid is completely dissolved, adding phosphoric acid, continuously stirring until the boric acid is uniformly mixed to prepare an addition solution, adding the addition solution and urea into the reaction kettle, stirring for 3-5min under the conditions that the rotating speed is 100-;
step A4: adding nanometer aluminum hydroxide, nanometer magnesium hydroxide and deionized water into a reaction kettle, stirring until the nanometer aluminum hydroxide and the nanometer magnesium hydroxide are completely dispersed, adding liquid paraffin and fatty glyceride, continuously stirring for 30-40min at the rotation speed of 5000-, adding the pre-modified vermiculite prepared in the step A3, continuously stirring for 20-30min, filtering to remove filtrate, drying a filter cake at the temperature of 120-130 ℃, adding the filter cake into deionized water until the filter cake is uniformly dispersed, adding the activated multi-walled carbon nano-tube prepared in the step A1, ultrasonic treatment is carried out for 30-50min under the condition of the frequency of 2-5MHz, filtering to remove the filtrate, and preserving the temperature of the filter cake for 2-3h at the temperature of 200-230 ℃ to obtain the flame-retardant filler.
3. The anti-halogenation inorganic fire-retardant floor according to claim 2, wherein: the mixed acid in the step A1 is prepared by mixing concentrated sulfuric acid and concentrated nitric acid in a volume ratio of 3:1, the mass fraction of the concentrated sulfuric acid is 75-80%, the mass fraction of the concentrated nitric acid is 70-75%, the dosage ratio of the filter cake to dimethyl sulfoxide is 5g:1mL, the dosage of dicyclohexylcarbodiimide is 45-50% of the mass of the filter cake, the concentration of the sodium chloride solution in the step A2 is 3-5mol/L, the concentration of the tetramethylammonium bromide solution is 1-1.5mol/L, the concentration of the hexadecyltrimethylammonium bromide solution is 2-5mol/L, the dosage of boric acid, phosphoric acid and urea in the step A3 is 1:1:1.8-2, the dosage of nano aluminum hydroxide and nano magnesium hydroxide in the step A4 is 1:1, and the dosage of liquid paraffin is 2-4% of the sum of the mass of the nano aluminum hydroxide and the nano magnesium hydroxide, the dosage of the fatty glyceride is 3-4% of the mass sum of the nano aluminum hydroxide and the nano magnesium hydroxide, the dosage of the pre-modified vermiculite is 5-8 times of the mass sum of the nano aluminum hydroxide and the nano magnesium hydroxide, and the dosage mass ratio of the filter cake to the activated multi-wall carbon nano tube is 2-2.5: 8.
4. The anti-halogenation inorganic fire-retardant floor according to claim 1, wherein: the waterproof additive is prepared by the following steps:
step B1: adding n-butyl titanate into isopropanol to mix until the n-butyl titanate is uniformly mixed, adding deionized water, stirring for 30-40min under the condition that the rotation speed is 120r/min, distilling for 10-15min under the condition that the temperature is 85-90 ℃, drying a substrate under the condition that the temperature is 60-80 ℃, and roasting for 2-3h under the condition that the temperature is 600 ℃ to prepare the nano titanium dioxide;
step B2: adding deionized water and sodium dodecyl benzene sulfonate into a reaction kettle, stirring at the rotation speed of 300-500r/min and the temperature of 50-60 ℃ until the sodium dodecyl benzene sulfonate is completely dissolved, adding fatty alcohol-polyoxyethylene ether and the nano titanium dioxide prepared in the step B1, stirring at the temperature of 70-80 ℃ for 10-15min, adding octamethylcyclotetrasiloxane, adjusting the pH value to 2-3, and stirring for 3-5h to prepare a mixed emulsion;
step B3: adding deionized water and silicon powder into a reaction kettle, stirring for 5-10min at the rotation speed of 800-1000r/min, adding sodium hydroxide, stirring for 6-8h at the temperature of 85-90 ℃, cooling to 40-45 ℃, standing for 10-15h to obtain silica sol, adding the silica sol and the mixed emulsion into the stirring kettle, and performing ultrasonic treatment for 2-3h at the frequency of 30-50kHz and the temperature of 35-40 ℃ to obtain the waterproof additive.
5. The anti-halogenation inorganic flame retardant floor according to claim 4, wherein: the volume ratio of the dosages of the n-butyl titanate, the isopropanol and the deionized water in the step B1 is 13-15:20:3-5, the mass ratio of the dosages of the deionized water, the sodium dodecyl benzene sulfonate, the fatty alcohol-polyoxyethylene ether, the nano titanium dioxide and the octamethylcyclotetrasiloxane in the step B2 is 10:2:2-2.5:1-1.3:1.5-2, and the mass ratio of the dosages of the deionized water, the silicon powder and the sodium hydroxide in the step B3 is 200:25: 0.15-0.2.
6. The method for processing the halogen-free inorganic flame retardant floor as claimed in claim 1, wherein the method comprises the following steps: the method specifically comprises the following steps:
step S1: adding magnesium chloride and deionized water into a reaction kettle, stirring until the magnesium chloride is completely dissolved to prepare a magnesium chloride solution with the Baume degree of 20-26, and standing for 20-25 h;
step S2: adding magnesium oxide, flame-retardant filler, waterproof additive and magnesium chloride solution into a stirring kettle, and stirring until the mixture is uniformly mixed under the condition that the rotating speed is 300-500r/min to prepare slurry;
step S3: laying a layer of non-woven fabric and a layer of alkali-free glass fiber fabric at the bottom of the mold, pouring the slurry prepared in the step S2 for molding, laying a layer of alkali-free glass fiber fabric and a layer of non-woven fabric, and drying at the temperature of 25-30 ℃ for 3-5 days to prepare a glass magnesium substrate;
step S4: and (4) moving the glass magnesium substrate prepared in the step (S3) into a curing chamber, curing for 20-30 days at the temperature of 45-55 ℃ and the humidity of 20-30%, moving the glass magnesium substrate out every 15-20h during curing, fumigating for 30-40min by using nitrogen loaded with 4-6% of trimethylaluminum by volume fraction, then placing into the curing chamber, and continuing to cure until the end to obtain the halogenated-resistant inorganic flame-retardant floor.
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